CN114656167A - Glass connecting method and device based on glass frit - Google Patents

Glass connecting method and device based on glass frit Download PDF

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Publication number
CN114656167A
CN114656167A CN202210281361.2A CN202210281361A CN114656167A CN 114656167 A CN114656167 A CN 114656167A CN 202210281361 A CN202210281361 A CN 202210281361A CN 114656167 A CN114656167 A CN 114656167A
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glass
frit
coating
cover plate
plate
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陈根余
钟沛新
程少祥
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Hunan University
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Hunan University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

The invention relates to a glass connecting method and a glass connecting device based on glass frit, wherein the connecting method is realized according to the following steps: step 1, coating glass frit on a glass substrate to obtain a glass frit coating; step 2, heating the glass substrate coated with the glass frit coating in a heating furnace, and removing organic impurities in the glass frit coating to obtain a heated glass substrate test piece; step 3, covering the glass cover plate on the test piece in the step 2, installing the test piece in a special device placed on a workbench, lifting the glass cover plate, and sintering the glass material coating in the step 2 by laser; and 4, pressing a glass cover plate downwards on the glass substrate test piece with the glass frit coating sintered by the laser in the step 3, and connecting the glass substrate and the glass cover plate. The frit coating is fully sintered by using laser, hidden defects in the coating are exposed, scrapping of devices caused in the laser welding process is avoided, formation of air holes in the subsequent laser welding process is effectively inhibited, the technological range of laser welding is expanded, the quality requirement on the frit coating is reduced, and the processing time is saved.

Description

Glass connecting method and device based on glass frit
Technical Field
The invention relates to a glass connection process, in particular to a glass connection method and device based on glass frit.
Background
The glass connection process is widely applied to the aspects of photoelectric device packaging, vacuum glass connection and the like. The glass frit is generally composed of glass frit, a solvent, a binder, and a filler.
The application of the glass-glass transparent material welding is mainly in two directions, one is to directly weld two pieces of glass by using ultrashort pulse laser; another research direction is to plate a layer of material which is opaque to laser wavelength on the lower glass plate, or add a layer of frit which is opaque to laser wavelength in the middle of the lower glass plate, so as to increase the absorption of laser energy at the interface of the two pieces of glass, and then transmit the absorbed energy to the upper and lower glass layers in a heat conduction manner, thereby realizing the welding of the glass and the glass. Currently, there is little research on laser welding of glass and glass using glass frit with a low softening temperature as an intermediate layer, and the glass joining process based on glass frit is generally divided into the following steps, (a) coating the glass frit on a substrate (usually by screen printing) to obtain a glass frit coating, (b) heat-treating (sintering) the glass frit-coated substrate, and heating the glass frit-coated substrate in a heating furnace to raise the temperature at least in the following three heating temperature stages: removing the organic solvent in the glass material coating, removing the adhesive, and pre-sintering to obtain a sintered layer, and (c) covering the cover plate, and connecting the substrate and the cover plate. The joining process is effected after the coating in the interlayer has been heated to the joining temperature.
Frit-based glass joining techniques typically achieve the joining process by locally melting the frit between the glass substrate and the glass cover plate by laser irradiation. Sintering is inevitably carried out before the laser bonding process using the glass frit as an intermediate layer. The most commonly used method of sintering is to place the entire coated glass substrate into a furnace and heat it according to a heating profile corresponding to the frit. Rui et al [1] (Rui T, et al. the effect of glass fraction depletion on encapsulation. International Conference on Electronic Packaging technique 2018.) studied the effect of different temperatures in the third stage of heating on the surface morphology of the sintered coating, with the flatter the surface, the better the bonding effect. Liu et al [2] (Liu Y, et al. glass fraction binding with controlled width and height using a two-step silicon etching process.J.Micromech.Microeng.2016; 26:035018) strictly controls the heating temperature curve to control the air hole to be minimum, improves the sintering process, changes the original heat preservation in the air of 60min at 450 ℃ into the heat preservation in the air for 30min, then heat preservation in the vacuum condition of the same temperature for 30min, and finally heats up to 500 ℃ and preserves the heat for 60min to reduce the generation of cracks in the glass coating. After sintering, the glass substrate and the cover plate are connected by a laser joining method. However, these methods require heating the glass substrate and the coating layer in a heating furnace until the pre-sintering is completed, and the heating time is generally more than 2 hours. To reduce porosity and cracking during joining requires more complicated heating and takes longer. Further, the presence of large-sized glass frit, impurities, residual gas, etc., in the glass frit is more or less insufficient for removal in the conventional sintering method, and as shown in fig. 16(a), a small amount of impurity-type pores is induced. Meanwhile, the frit coating obtained by the conventional sintering method needs to strictly control the input of laser energy in the welding process, otherwise, dense pores as shown in fig. 16(b) are easily generated, and the welding window is narrow. Before the welding process, the glass material coating is possibly polluted, and a large number of air holes appear after welding as shown in fig. 16(c), even can penetrate through the whole welding line, so that the welding quality is seriously influenced; in fig. 16(a), a small amount of impurity-induced voids are present in the frit, in fig. 16(b), dense voids are induced by excessive laser energy input, and in fig. 16(c), a large amount of voids are induced by contamination of the frit.
Disclosure of Invention
The glass connecting method and device based on the glass frit utilize laser to sinter the silk-screen glass frit coating, can effectively reduce the preparation process time, has better connecting effect of the prepared glass coating, and can also effectively reduce air holes and improve the welding process window and further the welding quality. On the basis, the device is used, and two steps of laser sintering and laser connection are completed on the same station, so that the production efficiency is further improved.
The invention aims to realize a glass connecting method based on glass frit by the following technical scheme, wherein a glass substrate and a cover plate are connected by using the glass frit, and the glass connecting method is characterized by comprising the following steps of:
step 1, coating glass frit on a glass substrate to obtain a glass frit coating;
step 2, heating the glass substrate coated with the glass frit coating in a heating furnace, and removing organic impurities in the glass frit coating to obtain a heated glass substrate test piece; step 3, after covering the glass cover plate on the test piece in the step 2, installing the test piece in a special device placed on a workbench, lifting the glass cover plate, and sintering the glass material coating in the step 2 by laser; and 4, pressing the glass cover plate downwards to connect the glass substrate and the glass cover plate on the glass substrate test piece which is sintered by the laser in the step 3 and is provided with the glass frit coating.
Further, if the thickness of the glass frit coating is less than 5 μm, in the step 2, the heating by the heating furnace sequentially comprises two heat preservation stages of removing the organic solvent in the glass frit coating and removing the binder in the glass frit.
Further, if the thickness of the glass material coating is more than or equal to 5 μm, the heating of the heating furnace sequentially comprises three heat preservation stages of removing the organic solvent in the glass material coating, removing the binder in the glass material and pre-sintering to obtain the sintering layer in the step 2.
Further, the technological parameters of the heat preservation stage for removing the organic solvent in the glass material are as follows: heating the glass substrate coated with the glass frit coating to 150 ℃ in the air, and keeping the temperature for 30min, wherein the temperature rising speed is 5 ℃/min.
Further, the technological parameters of the binder removing stage in the glass frit are as follows: and after the heat preservation stage of removing the organic solvent in the glass frit, continuously heating the glass substrate coated with the glass frit coating to 300 ℃, and preserving the heat for 30min at the temperature rising speed of 5 ℃/min.
Further, the process parameters of the stage of obtaining the sintering layer by pre-sintering are as follows: after the stage of removing the binder in the glass frit, the glass frit is continuously heated to 480 ℃ and is kept for 30 min.
Further, in the step 4, the glass substrate and the glass cover plate are connected by welding or by using a hot pressing method.
The invention also provides a device for carrying out laser sintering and laser welding on the same station based on the glass connecting method of the glass frit, which comprises a base, supporting blocks and four sets of air pressure control components fixed on four sides of the base; fixing the supporting block on the top of the base in a screw connection mode; the first cylinder, the second cylinder, the third cylinder and the fourth cylinder are respectively fixed on four sides of the base through threaded connection; the first pin, the second pin, the third pin and the fourth pin are fixed on four sides of the top of the supporting block respectively through holes reserved in the supporting block.
Furthermore, the first pressing plate penetrates through a gap between the first pin and the supporting block, the front end of the first pressing plate is in line contact with the glass cover plate, and the top of the first air cylinder is in line contact with a protruding part at the rear end of the first pressing plate; when the first cylinder is lifted, the front end of the first cylinder presses a first pressing plate through line contact, and the first pressing plate abuts against a first pin, so that the front end of the first pressing plate exerts pressure on the glass cover plate; when the first air cylinder is contracted, the first pressure plate is unloaded, the first pressure plate can be drawn out of the device, and after the first pressure plate is drawn out, the loading and unloading operation can be carried out at the position; the first cylinder, the first pressing plate and the first pin form a first set of air pressure control assembly.
Furthermore, a third pressing plate is placed between the third pin and the supporting block, the front end of the third pressing plate is in line contact with the glass cover plate and is hinged with a third cylinder through the pin, and the third pressing plate rotates around the pin; the third cylinder rises, and the front end of the third press plate is in line connection with the glass cover plate; when the third cylinder extends, the rear part of the third pressure plate is lifted through the pin, the third pressure plate props against the third pin, and the third pressure plate finishes pressure application on the glass cover plate; when the third cylinder contracts, the rear part of the third pressure plate is lowered through the pin, and the third pressure plate abuts against the protruding part of the supporting block to realize the lifting of the front end of the third pressure plate; when the third pressing plate applies pressure to the glass cover plate, the third sucker can complete adsorption on the glass cover plate by sucking air, and the adsorbed glass cover plate can ascend and descend along with the end of the third pressing plate; a third air cylinder, a third pressure plate, a third air pipe, a third sucker and a third pin form a third set of air pressure control assembly; in addition, the functions of the second set of air pressure control assembly and the fourth set of air pressure control assembly are the same as the functions of the third set of air pressure control assembly.
The invention has the beneficial effects that:
firstly, the silk-screen frit coating is sintered by laser, different processing technologies are formulated for the glass coatings with different thicknesses through deep research on the glass connection quality of the frit coatings with different thicknesses, the frit coatings are fully sintered by the laser, and large-particle frit, impurities, residual gas and the like contained in the glass coatings are further removed. The formation of air holes in the subsequent laser welding process can be effectively reduced, a larger process window can be obtained in the laser welding process, larger frit particles, impurities and the like can be tolerated, and the quality requirement on a frit coating is reduced; and the glass material coating after the laser sintering treatment can completely expose the hidden defects, so that the rejection of the whole device caused in the laser welding process is avoided.
Second, the present invention can replace the pre-sintering stage of low thickness frit coatings (<5 μm) in a furnace. The low-thickness glass material coating only needs to complete two-stage heat preservation stages of removing the organic solvent and the adhesive in a heating furnace, and is not pre-sintered in the heating furnace. Removing organic matters, directly processing by laser sintering, completing the complete sintering process of the low-thickness frit coating by utilizing a laser sintering process, improving the quality of the frit coating by acting laser on the frit coating, and then applying a glass cover plate for laser welding connection. The frit coating sintered by the method is not easy to form air holes in the laser sintering and subsequent laser welding connection processes, so that the air holes are effectively reduced, the connection effect of the coating after the laser sintering is finished is better, the range of a process window can be greatly improved, the time for sintering treatment in a heating furnace is saved, and the production efficiency is greatly improved.
Thirdly, in the sintering process of the glass material coating with higher thickness (more than or equal to 5 microns), due to the improvement of the coating thickness, if the heating sintering is carried out in a heating furnace, only two stages of heat preservation stages of removing the organic solvent and the adhesive are included, after the laser acts on the glass material coating, the energy can not be timely transmitted to the bottom of the glass material coating, so that the quality after the sintering is poor, and the laser welding method is difficult to be used for the subsequent laser welding treatment of the glass substrate and the glass cover plate. Therefore, in the heating process of the heating furnace of the frit coating with higher thickness (more than or equal to 5 microns), the glass substrate coated with the frit is sintered in the heating furnace to the pre-sintering stage, the glass substrate coated with the frit can be primarily sintered in the heating furnace for 30min until a sintered layer is obtained, then the glass substrate coated with the frit is taken out and is subjected to laser sintering, namely secondary sintering treatment is carried out by using laser, and finally the glass cover plate is covered for laser welding connection. The frit coating sintered by the method is also difficult to form air holes in the laser sintering and subsequent laser welding connection processes, the effect of the air holes can be effectively reduced, and the process window is enlarged. Although the primary sintering treatment is still required in the heating furnace, the sintering time in the heating furnace can be greatly shortened.
Fourthly, the glass prepared by the invention has the advantages of less welding seam air holes and good welding quality.
And fifthly, the device used by the invention completes two steps of laser sintering and laser connection on the same station, thereby further improving the production efficiency.
Drawings
The advantages of the above and/or additional aspects of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a graph of the heating temperature profile in a furnace for two thin and thick frit coatings according to the present invention;
FIG. 2 is a graph of the temperature of the center point of the weld during laser sintering according to the present invention over time;
FIG. 3 is a Differential Scanning Calorimetry (DSC) and Thermogravimetry (TG) plot of a frit according to the present invention;
FIG. 4 is a surface topography of a frit coating after pre-sintering of a low thickness frit coating in a furnace according to the present invention;
FIG. 5 is a surface topography of a frit coating after laser full sintering of a low thickness frit coating in accordance with the present invention;
FIG. 6 is a surface topography of a frit coating after direct laser full sintering of a high thickness frit coating in accordance with the present invention;
FIG. 7 is a surface topography of a frit coating after laser double through-sintering a high thickness frit coating in accordance with the present invention;
FIG. 8 is a photograph of a coaxial view of a laser fully sintered frit coating process according to the present invention;
FIG. 9 is a schematic cross-sectional view of a laser through-sintered frit coating process according to the present invention;
FIG. 10 is a photograph of a coaxial view of a laser welding process according to the present invention;
FIG. 11 is a schematic cross-sectional view of a laser welding process according to the present invention;
FIG. 12 is a weld morphology after sintering using only a heating furnace according to the present invention;
FIG. 13 is a weld profile after sintering using a laser according to the present invention;
FIG. 14 shows the appearance of a high-power welding seam after sintering in the heating furnace according to the present invention;
FIG. 15 is a high power weld profile after laser sintering in accordance with the present invention;
FIG. 16 is a graph of various porosity defects that occur during welding after sintering in a conventional manner according to the present invention;
FIG. 17 is a three-dimensional view of the device of the present invention;
fig. 18 is a cross-sectional view of the device of the present invention.
Wherein:
1-a fourth pressure plate, 2-a fourth air pipe, 3-a fourth pin, 4-a fourth sucker, 5-a fourth air cylinder and 6-a first pressure plate; 7-a first pin, 8-a first cylinder, 9-a base, 10-a supporting block, 11-a second cylinder; 12-second air pipe, 13-second pressing plate, 14-second pin, 15-third air cylinder, 16-third pressing plate, 17-third pin, 18-third air pipe 19-second suction cup, 20-third suction cup, 21-glass cover plate-, 22-glass substrate, 23-glass material coating and 24-pin.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
In the present invention, the terms "coating", "connecting", "sintering", etc. are to be construed broadly, and those skilled in the art can understand the specific meanings of the above terms in the present invention according to specific situations.
As shown in fig. 1, the temperature profile of the low thickness frit coating (<5 μm) in the furnace is a square mark point profile. The low-thickness glass material coating only passes through two steps of removing the organic solvent and the adhesive in the heating furnace, the heat preservation time of the two steps is 30min, and the temperature rising speed is 5 ℃/min. After the low-thickness frit coating layer processed by the heating furnace is cooled, the frit coating layer is subjected to laser sintering treatment using a laser beam. The time-dependent curve of the temperature of the center of the weld during the laser sintering process is shown in fig. 2. The frit can achieve a rapid temperature rise to 700 ℃ followed by a rapid temperature drop within 1 second. The surface appearance of the frit coating after laser complete pre-sintering observed under a metallographic microscope is shown in fig. 5, the surface of the coating is smooth, which indicates that the frit coating is fully melted in the laser sintering process, and the easily decomposed components and the impurities which can be removed at high temperature are fully removed. The Differential Scanning Calorimetry (DSC) and Thermogravimetry (TG) graphs (5 ℃/s) of the glass frits used in the present invention are shown in FIG. 3, and the optimal sintering temperature using a heating furnace is 340 to 480 ℃ by analyzing the graphs. After a number of process experiments, it was determined that the heating curve of the sintering process using the heating furnace is shown in the curve marked with a dot in fig. 1. The surface morphology of the glass frit coating after pre-sintering in the heating furnace observed under a metallographic microscope is shown in fig. 4, and the surface of the coating is rough, which indicates that the glass frit coating is not fully melted in the laser sintering process, and easily decomposed components, part of impurities and gas hidden in the glass frit coating cannot be fully removed. However, at this time, the sintering temperature of the frit in the heating furnace is not suitable to be increased, otherwise, a large amount of crystallization is easy to occur in the pre-sintering process of the frit coating, and the precipitated crystals exist in the frit coating as impurities, which affects the final welding quality.
For the high-thickness glass material coating (more than or equal to 5 mu m), the sintering process is directly carried out by adopting laser without heating to pre-sintering in a heating furnace (namely, the glass material coating does not experience the curve marked by the circle points in figure 1, but experiences the curve marked by the square points). The obtained weld surface appearance is shown in fig. 6, and vertical lines are generated on the weld surface due to excessive stress. The narrower striae disappear with re-melting of the frit during the welding process, but the wider striae inherit in the final weld. To avoid striae, the high-thickness frit coating is required to undergo a complete sintering profile in a furnace, and heated until pre-sintered to obtain a sintered layer. At this time, the frit was partially sintered, and after secondary sintering using the laser again, as shown in fig. 7, the surface of the frit coating was smooth and no striae appeared.
The frit coating sintered by the laser in the method can realize the full sintering of the frit, and the method is improved and not only can be suitable for the frit coating with low thickness, but also can be suitable for the frit coating with high thickness. The fully sintered glass material coating is not easy to form air holes in the subsequent process of covering a glass cover plate and performing laser welding connection, and has a wider window process range.
The apparatus used in the present invention will be described in detail below with reference to fig. 17 and 18.
As shown in fig. 17, this embodiment provides a device for laser sintering and laser welding at the same station, which comprises a base 9, a supporting block 10 and four sets of pressure control assemblies fixed on four sides of the base; the support block 10 is fixed on top of the base 9 by means of screw connections. The first cylinder 8, the second cylinder 11, the third cylinder 15 and the fourth cylinder 5 are respectively fixed on four sides of the base through threaded connection; the first pin 7, the second pin 14, the third pin 17 and the fourth pin 3 are respectively fixed on four sides of the top of the supporting block 10 through holes reserved in the supporting block 10.
As shown in the sectional view of fig. 18, in which the first presser plate 6 passes through the gap between the first pin and the support block 10, the front end of the first presser plate 6 is in line contact with the glass cover plate 21, and the top of the first cylinder 8 is in line contact with the rear-end projection of the first presser plate 6. When the first air cylinder 8 is lifted, the front end of the first air cylinder extrudes the first pressing plate 6 through line contact, and the first pressing plate 6 is propped against the first pin 7, so that the front end of the first pressing plate 6 applies pressure to the glass cover plate 21. When the first cylinder 8 contracts, the first pressing plate 6 is under the action of force unloading, the device can be drawn out, and the device is a loading and unloading position of a glass plate, and after the first pressing plate 6 is drawn out, loading and unloading operations can be carried out at the position.
The first air cylinder 8, the first pressure plate 6 and the first pin 7 form a first set of air pressure control assembly.
The third pressing plate 16 is placed between the third pin 17 and the supporting block 10, the front end of the third pressing plate is in line contact with the glass cover plate 21, the third pressing plate 16 is hinged with the third air cylinder 15 through the pin 24, and the third pressing plate 16 can rotate around the pin 24.
The third cylinder 15 is raised and the front end of the third presser plate 16 is in line contact with the glass cover plate 21. When the third air cylinder 15 extends, the rear part of the third pressing plate 16 is lifted through the pin 24, the third pressing plate 16 abuts against the third pin 17, and the third pressing plate 16 finishes applying pressure to the glass cover plate 21. When the third air cylinder 15 contracts, the rear part of the third pressing plate 16 is lowered through the pin 24, and the third pressing plate 16 abuts against the protruding part of the supporting block 10, so that the front end of the third pressing plate 16 is lifted.
The third suction cup 20 is inserted into the hole in the middle of the front end of the third pressing plate 16 through the cylindrical joint on the suction cup, so that the third suction cup 20 and the third pressing plate 16 are fixed together. The third suction cup 20 is made of rubber and has certain elasticity, and is compressed after being stressed, so that the length is shortened, and the suction cup slightly protrudes out of the third pressing plate 16 when not stressed. The third suction pipe 18 is a rubber hose and is inserted into an air guide position on the upper part of the third suction cup 20. When the third pressing plate 16 presses the glass cover plate 21, the third suction cups 20 are forced to contract flush with the front end projections of the third pressing plate 16 while being in full contact with the glass cover plate 21. At this time, the air pipe 18 is evacuated, negative pressure is generated in the third suction cup 20, the glass cover plate 21 and the third suction cup 20 can be sucked together, and after the suction is completed, the glass cover plate 21 can move up and down along with the front end of the third pressing plate. The third air cylinder 15, the third pressure plate 16, the third air pipe 18, the third suction cup 20 and the third pin 17 form a third set of air pressure control assembly.
The connection mode among the second air cylinder 11, the second pressing plate 13, the second air pipe 12, the second suction cup 19 and the second pin 14 and the connection mode among the fourth air cylinder 5, the fourth pressing plate 1, the fourth air pipe 2, the fourth suction cup 4 and the fourth pin 3 are the same as the connection mode among the third air cylinder 15, the third pressing plate 16, the third air pipe 18, the third suction cup 20 and the third pin 17 in the third set of air pressure control assembly, and respectively form a second set of air pressure control assembly and a fourth set of air pressure control assembly.
Example 1
The laser sintering method in the embodiment comprises the following steps:
step 1: the glass substrate is ultrasonically cleaned by a mixed solution of distilled water and a cleaning agent.
Step 2: the glass slurry is coated on the glass substrate in a silk-screen printing mode. Wherein, two screen printing plates are adopted, and the film thickness is 10 mu m. The width of the silk-screen pattern is 0.8 mm. And finally, the thickness of the coating is 4-5 mu m, and the low-thickness glass frit coating is obtained.
And 3, step 3: the heating stage of the low-thickness frit coating in a heating furnace is divided into two sections, the heating furnace directly heats the glass substrate coated with the coating to 150 ℃ in the air, the temperature is kept for 30min, and the organic solvent is removed; heating to 300 deg.C, maintaining the temperature for 30min, and removing the adhesive. The heating furnace temperature rise curve is shown in FIG. 1.
And 4, step 4: and drawing out the first pressing block 6, contracting the first cylinder 8, the second cylinder 11, the third cylinder 15 and the fourth cylinder 5, covering the glass substrate 22 treated by the heating furnace with a glass cover plate 21, placing the test piece into the groove on the supporting block 10 from the position of the original first pressing block 6, and installing the device on a laser processing platform, wherein the continuous laser used by the platform is semiconductor laser with the wavelength of 915 nm. The focal length of the laser head is 150mm, and the diameter of a light spot at the focal point is 300 mu m. The process parameters used for laser sintering were set as: defocusing amount is-15 mm, laser scanning speed is 0.1m/min, and laser power is 28W. And (3) putting the first pressing plate 6 back to the original position, extending the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 to enable the suction cup to be attached to the glass cover plate 21, exhausting air from the second air pipe 12, the third air pipe 18 and the fourth air pipe 2, and enabling the suction cup to adsorb the glass cover plate 21. And contracting the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 to lift the second pressing plate 13, the third pressing plate 16 and the fourth pressing plate 1, simultaneously lifting the glass cover plate 21 adsorbed by the air cylinders to keep a sufficient distance between the glass cover plate 21 and the glass frit coating 23 on the glass substrate 22, and performing final laser sintering treatment on the glass frit coating by the laser penetrating through the glass cover plate 21. After treatment, the first air cylinder 8, the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 are simultaneously extended, so that the front ends of the first pressing plate 6, the second pressing plate 13, the third pressing plate 16 and the fourth pressing plate 1 are pressed downwards, and after the glass cover plate 21 is in full contact with the glass material coating 23, laser welding treatment is carried out on the same device. After welding, the second air pipe 12, the third air pipe 18 and the fourth air pipe 2 are blown with air, the first air cylinder 8, the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 are contracted, the second pressing plate-413, the third pressing plate 16 and the fourth pressing plate 1 are lifted upwards, the first pressing plate 6 is unloaded, the first pressing plate 6 is pulled out, and a welded finished product is taken out.
Example 2
The laser sintering method in the embodiment comprises the following steps:
step 1: the glass substrate was ultrasonically cleaned with a mixed solution of distilled water and a cleaning agent.
Step 2: the glass slurry is coated on the glass substrate in a silk-screen printing mode. Wherein, two screen printing plates are adopted, and the thickness of the screen printing plate is 25 mu m. The width of the silk-screen pattern is 0.8 mm. And finally, the thickness of the coating is 8-10 mu m, and the high-thickness glass frit coating is obtained.
And step 3: the heating stage of the high-thickness glass material coating in the heating furnace is divided into three sections: organic solvent removal, binder removal and pre-sintering. The heating curve is shown in FIG. 1, after removing the organic solvent and the binder, heating to 480 deg.C and maintaining for 30min, and sintering.
And 4, step 4: the first pressing plate 6 is drawn out, the first air cylinder 8, the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 are contracted, the glass cover plate 21 is covered on the test piece glass substrate 22 processed by the heating furnace, the test piece is placed in the groove on the supporting block 10 from the position of the original first pressing plate 6, the device is installed on a laser processing platform, and continuous laser used by the platform is semiconductor laser with the wavelength of 915 nm. The focal length of the laser head is 150mm, and the diameter of a light spot at the focal point is 300 mu m. The process parameters used for laser sintering were set as: defocusing amount is-15 mm, laser scanning speed is 0.1m/min, and laser power is 23W. And (3) putting the first pressing plate 6 back to the original position, extending the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 to enable the suction cup to be attached to the glass cover plate 21, exhausting air from the second air pipe 12, the third air pipe 18 and the fourth air pipe 2, and enabling the suction cup to adsorb the glass cover plate 21. And contracting the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 to lift the front ends of the second pressing plate 13, the third pressing plate 16 and the fourth pressing plate 1, simultaneously lifting the glass cover plate 21 adsorbed by the air cylinders to keep a sufficient distance between the glass cover plate 21 and the frit coating 23 on the glass substrate 22, and performing final laser sintering treatment on the frit coating by the laser through the glass cover plate 21 by using proper process parameters. After the laser sintering treatment, the first air cylinder 8, the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 are simultaneously extended, and the first pressing plate 6, the second pressing plate 13, the third pressing plate 16 and the fourth pressing plate 1 are pressed downwards, so that the glass cover plate 21 is in full contact with the glass material coating 23, and then laser welding treatment is carried out on the same laser processing platform device. After welding, the second air pipe 12, the third air pipe 18 and the fourth air pipe 2 blow air, the glass cover plate 21 is not adsorbed any more, the first air cylinder 8, the second air cylinder 11, the third air cylinder 15 and the fourth air cylinder 5 are contracted, the front ends of the second pressing plate 13, the third pressing plate 16 and the fourth pressing plate 1 are lifted upwards, the first pressing plate 6 is unloaded, the first pressing plate 6 is drawn out, and a welded finished product is taken out.
In the above embodiment, since the frit itself is not a homogeneous material, there is a possibility that impurities or frit particles in a certain portion of the frit coating after screen printing may be large, which may cause large bubbles to be formed during laser sintering. After the larger bubbles escape, small pits can form on the surface of the frit coating, as can be seen by the small white dots in fig. 8. Wherein: fig. 8(a) t is 10.07s, fig. 8(b) t is 10.10s, and fig. 8(c) t is 10.20 s; while larger pores will form a ring-shaped plateau on the frit coating surface as shown by the white dots in the circle in fig. (8c) of the axial view. The cross-sectional view of the whole bubble overflow process is schematically shown in fig. 9, wherein fig. 9(a) separates out the pores, fig. 9(b) forms the pits, and fig. 9(c) forms the annular bosses.
Pits or annular lands may form after laser sintering, which may appear to hinder the joining process. Fig. 10 shows the joining process of the test pieces after laser sintering, where t in fig. 10(a) is 11.01s, t in fig. 10(b) is 11.09s, and t in fig. 10(c) is 11.13 s; the white spots of the frit coating in fig. 10a are small pits, the ones in the circles are ring-shaped projections, and the dark black areas are the connecting portions of the molten frit and the upper glass substrate. As shown in the schematic diagram 10(a), the glass upper substrate is bent and deformed downward. As shown in fig. 10(b), the small pits were directly covered with the molten frit and the annular lands melted before the leading edge of the molten frit reached. As shown in fig. 11(b), the annular boss forms the color center, has a laser absorption stronger than the peripheral frit, melts and wets the glass upper substrate by the edge of the laser beam, and a gap occurs. Fig. 10(c) shows that the fused annular boss is covered by the fusion front. That is, as shown in the schematic view of fig. 11(c), the gap portion is completely filled with the molten glass frit, in which: FIG. 11(a) is a step of precipitating pores, FIG. 11(b) is a step of removing the fine pores and remelting the projections, and FIG. 11(c) is a step of filling the gaps; therefore, after the laser sintering process is used, the final laser glass welding forming cannot be influenced by larger impurities or glass frit particles in the glass frit coating.
As shown in fig. 12, in the conventional process, the frit coating that is sintered only in the heating furnace has many fine pores in the middle of the weld after laser welding. As shown in fig. 13, after the glass frit coating layer treated by the laser sintering process was connected to the glass substrate and the cover plate by laser welding, the pores were hardly visible, and the weld was well formed. After the laser welding power is increased by 2W, the surface of the welded joint of the frit coating which is sintered only in the heating furnace is as shown in fig. 14, and the width of the welded joint is greatly expanded compared with that in fig. 12, and the number of the pores is increased. The surface of the weld joint after the laser welding power is increased by 2W by using the laser sintered frit coating is shown in FIG. 15, the width of the weld joint is also wider, and only a small amount of micro pores appear at two ends of the weld joint. Therefore, the frit coating processed by the laser sintering method can adapt to a larger process window range in the subsequent laser welding process.
While the principles of the invention have been described in detail in connection with the preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing embodiments are merely illustrative of exemplary implementations of the invention and are not limiting of the scope of the invention. The details in the examples are not to be construed as limitations on the scope of the invention, and any obvious modifications, equivalent alterations, simple substitutions, etc. based on the technical solution of the present invention are intended to fall within the scope of the present invention without departing from the spirit and scope of the present invention.

Claims (10)

1. A glass connecting method based on glass frit, which connects a glass substrate and a cover plate by using the glass frit, is characterized by comprising the following steps:
step 1, coating glass frit on a glass substrate to obtain a glass frit coating;
step 2, heating the glass substrate coated with the glass frit coating in a heating furnace, and removing organic impurities in the glass frit coating to obtain a heated glass substrate test piece;
step 3, after covering the glass cover plate on the test piece in the step 2, installing the test piece in a special device placed on a workbench, lifting the glass cover plate, and sintering the glass material coating in the step 2 by laser;
and 4, pressing a glass cover plate downwards on the glass substrate test piece which is sintered by the laser in the step 3 and is provided with the glass material coating, and connecting the glass substrate and the glass cover plate.
2. The method for joining glass based on glass frit according to claim 1, wherein the thickness of the glass frit coating is less than 5 μm, and the heating in the heating furnace in step 2 comprises two heat preservation stages of removing the organic solvent in the glass frit coating and removing the binder in the glass frit.
3. The method for joining glass based on glass frit according to claim 1, wherein the thickness of the glass frit coating is 5 μm or more, and the heating in the heating furnace in step 2 sequentially comprises three heat preservation stages of removing the organic solvent in the glass frit coating, removing the binder in the glass frit, and pre-sintering to obtain the sintered layer.
4. The method for joining glass based on frit according to claim 1, wherein the process parameters of the incubation period for removing the organic solvent in the frit are as follows: heating the glass substrate coated with the glass frit coating to 150 ℃ in the air, and keeping the temperature for 30min, wherein the temperature rising speed is 5 ℃/min.
5. The method for joining glass based on glass frit according to claim 3 or 4, wherein the process parameters of the binder removal stage in the glass frit are: and after the heat preservation stage of removing the organic solvent in the glass frit, continuously heating the glass substrate coated with the glass frit coating to 300 ℃, and preserving the heat for 30min at the temperature rising speed of 5 ℃/min.
6. The method for joining glass based on glass frits according to claim 3 or 4, wherein the pre-sintering to obtain a sintered layer stage process parameters are: after the stage of removing the binder in the glass frit, the glass frit is continuously heated to 480 ℃ and is kept for 30 min.
7. The method for joining glass frit-based glass plates according to claim 1, wherein in step 4, the glass substrate plate and the glass cover plate are joined by means of soldering or by means of thermocompression.
8. An apparatus for performing laser sintering and laser welding at the same station by using the glass connection method based on frit according to claim 1, comprising a base (9), a supporting block (10) and four sets of air pressure control components fixed on four sides of the base; fixing the supporting block (10) on the top of the base (9) in a screw connection mode; the first cylinder (8), the second cylinder (11), the third cylinder (15) and the fourth cylinder (5) are respectively fixed on four sides of the base through threaded connection; the first pin (7), the second pin (14), the third pin (17) and the fourth pin (3) are fixed on four sides of the top of the supporting block (10) through holes reserved in the supporting block (10) respectively.
9. The apparatus of claim 8, wherein: the first pressing plate (6) penetrates through a gap between the first pin and the supporting block (10), the front end of the first pressing plate (6) is in line contact with the glass cover plate (21), and the top of the first air cylinder (8) is in line contact with a protruding part at the rear end of the first pressing plate (6); when the first air cylinder (8) is lifted, the front end extrudes the first pressing plate (6) through line contact, the first pressing plate (6) is propped against the first pin (7), and the pressure of the front end of the first pressing plate (6) on the glass cover plate (21) is applied; when the first cylinder (8) contracts, the first pressure plate (6) is unloaded, the first pressure plate (6) can be drawn out of the device, and after the first pressure plate (6) is drawn out, the loading and unloading operation can be carried out at the position; the first air cylinder (8), the first pressing plate (6) and the first pin (7) form a first set of air pressure control assembly.
10. The apparatus of claim 8, wherein: the third pressing plate (16) is placed between the third pin (17) and the supporting block (10), the front end of the third pressing plate is in line contact with the glass cover plate (21), the third pressing plate is hinged with the third air cylinder (15) through the pin (24), and the third pressing plate (16) rotates around the pin (24); the third cylinder (15) rises, and the front end of the third press plate (16) is connected with the glass cover plate (21) by a wire; when the third air cylinder (15) extends, the rear part of the third pressure plate (16) is lifted through the pin (24), the third pressure plate (16) props against the third pin (17), and the third pressure plate (16) completes the pressure application on the glass cover plate (21); when the third air cylinder (15) contracts, the rear part of the third pressure plate (16) is lowered through the pin (24), and the third pressure plate (16) is propped against the convex part of the supporting block (10) to realize the lifting of the front end of the third pressure plate (16); when the third pressing plate (16) applies pressure to the glass cover plate (21), the third sucker (20) sucks air to complete adsorption of the glass cover plate, and the adsorbed glass cover plate can ascend and descend along with the front end of the third pressing plate (16); a third air cylinder (15), a third pressure plate (16), a third air pipe (18), a third sucker (20) and a third pin (17) form a third set of air pressure control assembly; in addition, the functions of the second set of air pressure control assembly and the fourth set of air pressure control assembly are the same as the functions of the third set of air pressure control assembly.
CN202210281361.2A 2022-03-21 2022-03-21 Glass connecting method and device based on glass frit Pending CN114656167A (en)

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CN105330177A (en) * 2015-11-27 2016-02-17 中国建筑材料科学研究总院 Method for preparing sealing glass prefabricated part by selective laser sintering
CN106587581A (en) * 2016-12-11 2017-04-26 大连哈尼比科技有限公司 Glass fusion bonding method, as well as manufacturing method and manufacturing equipment of vacuum glass

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Publication number Priority date Publication date Assignee Title
CN102112406A (en) * 2008-05-30 2011-06-29 康宁股份有限公司 Method for sintering frit to glass plate
CN102066277A (en) * 2008-06-11 2011-05-18 浜松光子学株式会社 Fusion-bonding process for glass
CN102690044A (en) * 2011-03-21 2012-09-26 上海微电子装备有限公司 Packaging method
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Application publication date: 20220624