Disclosure of Invention
The invention aims to provide an efficient full-tempered vacuum glass production process to solve the technical problem that vacuum glass produced by the existing process has a large air leakage risk.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of high-efficiency fully tempered vacuum glass comprises the following steps:
(1) film coating: coating a film layer made of a metal material on the edge of one side surface of the glass plate;
(2) solder fixation and support post arrangement: the glass sheets comprise a first glass sheet and a second glass sheet; placing the first glass plate in a state that the film layer is upward, fixing the solder on the film layer of the first glass plate, and arranging the support columns on the upper surface of the first glass plate;
(3) pre-exhausting; (4) getter activation and lamination; (5) and (6) heat treatment.
The principle and the advantages of the scheme are as follows: according to the scheme, the film coating treatment is firstly carried out on the edge of the glass plate, then the welding flux is directly fixed on the film layer of the first glass plate, the supporting columns are arranged on the first glass plate through automatic equipment, then pre-exhausting, getter activating, sheet combining and heat treatment are carried out, and finally the vacuum glass product with good quality and long service life is obtained.
The scheme adopts a solder pre-welding means, and comprehensively improves the sealing degree, the service life and the like of the vacuum glass compared with the traditional process. The prior art generally places solder directly on the metallization layer (film layer), and the solder is prone to positional displacement during subsequent transportation. The solder is arranged in the metalized layer area, the solder is usually a metal alloy material and is an independent solid material, particularly when large glass is processed, the solder is not flat, the glass metal area is not flat, and when the glass is laminated, the solder is simultaneously sealed and fixed on the upper glass plate and the lower glass plate, so that a cavity is easily generated between the solder and the glass plates, and the risk of defects and even air leakage of the sealed area exists. The scheme prewelds the welding flux on the metal film of one piece of glass, so that the contact surface between the film and the welding flux can be improved, the sealing performance can be improved, and the service life of the product can be prolonged.
Further, in the step (1), a coating film layer is coated on the edge of one side surface of the glass plate in a magnetic sputtering, screen printing, ink-jet printing or coating mode; the film layer is made of at least one of silver, copper, aluminum, cobalt and nickel. The preparation method and the material of the film layer can realize the effective sealing of the vacuum glass. Among them, the magnetic sputtering method is most preferable. Compared with the traditional method for forming the metallization layer in the toughening or thermal strengthening process, the method has the advantages that the phenomenon that the glass is heated unevenly due to the existence of metal slurry on the edge part and the phenomena that the toughened glass is uneven and the glass is broken in the sealing process due to the unevenness of the glass are avoided.
Further, in (2), the shape of the supporting column is cylindrical, drum-shaped, square or circular; the preparation method of the support column comprises the following steps: the laser cutting, the water jet cutting or the water sand cutting is carried out on the base material with the thickness of 0.1-0.5mm and the smooth surface.
In the prior art, paste glass material is selected as a support column and is placed on one of glass substrates in a printing mode, firstly, a dot-shaped raised support column with a certain thickness is difficult to form in the printing mode, the thickness of the support column of the vacuum glass is usually 0.1mm-0.5mm, the height consistency of all the support columns on a single substrate is difficult to ensure even in a multi-time printing mode, and the uneven height can cause uneven stress on each support point of the vacuum glass, so that the overall strength of the product is reduced.
In this technical scheme, select for use the sheet metal of certain width, thickness is unanimous with support column thickness, puts into laser cutting machine (or conventional cutting equipment among other prior art), sets for the stroke and sets for circular, square or other settlement shapes, puts into magnetic grinding equipment again and carries out polishing treatment, takes out the support column and washs the stoving, puts into the support column at last and puts and carry out automatic putting in the material storage disc of equipment. The support column prepared according to the process is smoother, and the quality of the vacuum glass is improved.
Further, the base material is stainless steel 304, iron, tungsten steel, PV, Teflon, glass, ceramic or microcrystalline glass. The support column prepared by using the base material made of the material has proper strength and can effectively support two glass plates.
Further, in (2), the solder is in the form of paste, filament, or sheet; the solder is made of tin, lead, silver, copper, indium or nickel. The solder made of the material can effectively seal two glass plates of the vacuum glass to form a vacuum space.
Further, the method for fixing the solder on the film layer comprises the following steps: melting, hot pressing or argon arc welding, and the fixing process is carried out in an inert gas or vacuum environment. The methods of melting, hot pressing or argon arc welding and the like are conventional metal welding methods in the prior art, and welding operation is carried out in inert gas or vacuum environment, so that the metal film layer and the welding flux can be prevented from being oxidized, and the quality of the vacuum glass is improved.
The traditional process is to directly place a metal sheet or strip at the film layer, and the inventor also finds that the contact effect between the solder and the film layer is poor after adopting the method. The inventor further adopts a mode of prewelding to reduce the occurrence of the situations, and also adopts various modes when prewelding, so that the method of melting, hot pressing or argon arc welding and the like can realize better effect, and the solder can fully react with the metal film layer. When the laser prewelding mode is adopted, the power is difficult to control, so that multiple failures are caused.
Further, in (3), the glass plate is treated for 3 to 10min by means of electron irradiation or plasma in an environment of a vacuum degree of 1Pa, and is heated to 50 to 200 ℃.
The method comprises the steps of firstly carrying out electron bombardment on two glass plates, removing organic matters on the surface of the glass through plasma under a certain vacuum degree to play a cleaning role, simultaneously enabling high-speed electrons to collide with gas molecules physically adsorbed on the surface of the glass to enable the gas molecules to have a large amount of kinetic energy to be separated from the surface of the glass, and increasing the temperature of the surface of the glass to accelerate the evaporation of water vapor on the surface of the glass. The electron bombardment and the heat radiation are cooperated to increase the service life of the vacuum glass. After the plasma treatment is carried out for 3-10min, the treatment effect reaches the optimal level, the treatment time is continuously increased, and the effect is not improved. If the amount is less than this range, the treatment effect is poor, i.e., the vacuum life of the final product is maintained for a short time.
Further, in (4), the first glass plate is placed with the film layer facing upward, and the second glass plate is placed with the film layer facing upwardThe glass plate is conveyed into a vacuum degree of 10 in a state that the film layer faces downwards-4A getter is placed on the first glass plate, and the second glass plate is positioned right above the first glass plate; heating the getter to 500-1200 ℃, then placing the second glass plate on the first glass plate, and finally sealing and fixing the solder and the film layer of the second glass plate to obtain the vacuum glass after sealing.
The scheme of piece is closed in vacuum environment to this scheme adoption, is different from the technical scheme of the prior art piece of closing and evacuation again, has solved the operation degree of difficulty that traditional mode closed the piece earlier and then formed the vacuum, has simplified the process, has reduced the processing degree of difficulty of equipment in vacuum environment, promotes the uniformity of vacuum glass product vacuum, and production efficiency is higher.
According to the scheme, the getter is heated to 500-1200 ℃ before the sheet combination, so that the getter is activated. The temperature is too low, and the activation time is too long; the temperature is too high, the material used by the equipment mechanism is more strict, and the equipment cost is higher. Conventional getter activation is done after the final product is formed, and the getter is again outgassed during the activation process. The process is activated in a vacuum environment, and the generated gas is directly pumped away by a vacuum pump so as to improve the vacuum degree of a vacuum glass product.
10-4Pa is the optimal vacuum degree value of the vacuum degree of the vacuum glass, and the acquisition time of the over-high vacuum degree is longer, which is not beneficial to the continuity of production; if the vacuum degree is too low, the initial vacuum degree of the vacuum glass is low, and the quality of subsequent products is poor.
Further, in the step (4), the vacuum glass after sealing is subjected to heat treatment at the temperature of 100 ℃ and 230 ℃ to obtain a finished vacuum glass product. And carrying out heat treatment on the vacuum glass after sealing, so that the stress between the solder and the metal film layer is released, and the probability of self-explosion of the vacuum glass and tearing of the metal film layer are reduced. The softening effect is poor and the stress release is insufficient due to the over-low temperature; too high a temperature will cause the sealing material to melt again resulting in seal failure.
Furthermore, a groove for placing a getter is formed in the first glass plate. The grooves for placing the getters are arranged, so that the getters can be prevented from scattering around the glass plate in the process of moving along with a production line, and further, the waste of materials and the pollution to the production environment are avoided.
Detailed Description
Reference numerals in the drawings of the specification include: the device comprises a first glass plate 1, a second glass plate 2, a solder 3, a support column 4, a vacuum gap layer 5, a glass deep processing device 6, a metal film forming device 7, a solder pre-welding device and getter placing device 8, a solid support manufacturing device 9, a distributing device 10, a glass pre-exhausting device 11, a vacuum attaching, sealing and activating device 12, a vacuum glass softening device 13 and a vacuum glass performance detection device 14.
Example 1
Referring to fig. 1, the vacuum glass of the prior art includes a first glass plate 1 and a second glass plate 2 parallel to each other, edges of the first glass plate 1 and the second glass plate 2 are sealed by a solder 3, and a space formed between the first glass plate 1 and the second glass plate 2 is evacuated to form a vacuum gap layer 5. In order to avoid collapse between the first glass plate 1 and the second glass plate 2 under the action of atmospheric pressure, a number of support pillars 4 are provided between the first glass plate 1 and the second glass plate 2.
A production process of high-efficiency fully tempered vacuum glass comprises the following steps:
s1: and carrying out conventional cutting, edging, slotting, cleaning and toughening operations on the glass sheet to obtain the pretreated glass. Wherein the glass raw sheet can be produced by a conventional float process. The purpose of notching the glass blank is to make room for the subsequent storage of getters (prior art conventional zircaloy getters). Since the vacuum glass is made of two pieces of glass, at least one of the pieces of glass needs to be selected for grooving (for example, grooving on the first glass plate 1). The shape of the slot can be round, square, oval, diamond, long strip and other shapes. The grooving mode can be a conventional grooving mode in the prior art, for example, grooving by a numerical control milling machine, water milling, water sand milling and etching to form a customized shape.
And (3) performing film removal operation on the pretreated glass, and removing the film carried on the surface of the edge of the glass by adopting conventional modes such as laser, grinding wheel, water sand and the like to obtain the glass to be coated.
S2: and coating a metal material on the surface of the edge of the glass to be coated by adopting a magnetic sputtering method. Other coating methods known in the art, such as screen printing, ink jet printing, and coating, can of course be used. And after the edge of the glass to be coated is covered with a metal film layer, baking the film layer to finally obtain the metal coated glass with the film layer coated on the edge. More specifically, the film layer is at least one layer, the composition of the film layer is one of silver, copper, aluminum, cobalt and nickel, metal particles are deposited on the surface of the edge of the glass to be coated by using a conventional magnetic sputtering method in the prior art, and the deposition thickness is 10-50 μm (preferably 10-15 μm).
S3: the support pillars 4 are placed on a glass substrate, which is referred to as the first glass plate 1 in this embodiment for convenience of explanation, and the first glass plate 1 is placed with its groove in which the getter is placed facing upward and its film facing upward. The support column 4 is cylindrical, drum-shaped, square or circular, and can be formed by processing a metal plate in a laser cutting or water-jet cutting mode.
S4: the solder 3 is fixed above the film layer, and the getter is synchronously placed in the groove reserved in the previous process. The solder 3 can be paste, thread or sheet metal materials such as tin, lead, silver, copper, indium, nickel and the like, the solder 3 is integrated with the metal film layer in advance in a melting, hot pressing or argon arc welding mode, the whole process can be carried out in an inert gas or vacuum environment, the embodiment specifically selects a 1Pa vacuum environment, and the solder 3 is welded on the film layer in a mode of melting the solder 3 through resistance heating.
The support posts 4 and the solder 3 in the above steps are visually inspected, and the process is completed by the aid of a camera, so that the arrangement condition of the support posts 4 and the forming effect of the solder 3 are detected. And adding a repairing machine after S3 or S4, and if a problem is detected, performing manual repairing or mechanical automatic repairing.
S5: and synchronously conveying the first glass plate 1 and the second glass plate 2 into a vacuum chamber for pre-exhausting, wherein the first glass plate 1 is positioned below and horizontally placed, and the second glass plate 2 is positioned right above the first glass plate 1 and also horizontally placed. The membranous layer of first glass board 1 faces up, and the membranous layer of second glass board 2 faces down, and the membranous layer of two places sets up relatively.
The pre-exhaust mode adopts the conventional electron radiation or plasma mode in the prior art to treat the glass surface, and the embodiment specifically adopts the plasma treatment mode, the treatment time is 3-10min, the vacuum degree of the vacuum chamber is 1Pa, and the power is 30W. The medium for plasma treatment can be helium, argon, hydrogen or nitrogen, and nitrogen is specifically used in the scheme. A heat source with adjustable heat radiation range is arranged in the vacuum chamber, and can heat the first glass plate 1 and the second glass plate 2 to 50-200 ℃.
S6: at a vacuum degree of 10-4Activating a getter in a vacuum chamber of Pa, wherein the getter is activated before sheet combination, and the getter is heated to 500-1200 ℃ by using laser or ultrasonic and the like (preferably to 800-1000 ℃ with the heating time controlled within 10 s), so as to complete the activation. Then, the first glass plate 1 and the second glass plate 2 are laminated. The second glass plate 2 can be grasped by means of static electricity, viscous liquid, adhesion and the like and slowly placed on the first glass plate 1, so that the vacuum attaching process is realized. And the welding flux 3 is sealed with the film layer of the second glass plate 2 by adopting modes of heat radiation, resistance heating, high-frequency integral heating and the like, and the welding flux 3 is fused and sealed with the film layer of the second glass plate 2 by adopting a resistance heating method in the embodiment. And after the integral sealing of the vacuum glass is finished, the vacuum glass after sealing is formed.
S7: the sealing area of the vacuum glass after sealing is again subjected to heat treatment, or the whole vacuum glass is subjected to heat treatment, and the former is adopted in the embodiment. The heat treatment temperature range is 100-. The heat treatment time is usually 5-30min, and then natural cooling is carried out. The vacuum glass finished product is finally obtained by the step.
S8: and (3) carrying out online detection on the performance of the vacuum glass, and judging whether the vacuum glass is qualified or not, wherein detection indexes comprise heat transfer coefficient detection, stress spot detection and sound insulation detection.
Example 2:
the process of example 1 was carried out in the high efficiency all tempered vacuum glass production line of this example as shown in figure 2. The production line comprises a glass deep processing device 6, a metal film forming device 7, a solid support manufacturing device 9, a distributing device 10, a solder pre-welding device, a getter placing device 8, a glass pre-exhausting device 11, a vacuum laminating and sealing activation device 12, a vacuum glass softening device 13 and a vacuum glass performance detection device 14 which are sequentially arranged.
The glass deep processing device 6 comprises an automatic sheet feeding machine, a conveying roller way, an edge grinding and chamfering device, a cleaning device and glass toughening equipment; the metal film forming device 7 comprises a vacuum chamber, a vacuum pump, an ion evaporation and sputtering source, a cooling system and an industrial control system. The process step S1 is performed in the glass deep processing apparatus 6, the process step S2 is performed in the metal film forming apparatus 7, the process step S3 is performed in the placement apparatus 10, and the support pillars 4 are formed in the solid support forming apparatus 9. The process step S4 is performed in the solder pre-soldering device and the getter placing device 8, the process step S5 is performed in the glass pre-exhausting device 11, the process step S6 is performed in the vacuum sealing activation device 12, the process step S7 is performed in the vacuum glass softening device 13, and the process step S8 is performed in the vacuum glass performance detection device 14.
The support pillars 4 are formed in the solid support forming device 9, and a base material having a thickness of 0.1 to 0.5mm is cut into a predetermined shape by means of laser, water jet, water sand cutting or the like. The material of the substrate can be metal material, including stainless steel 304, iron plate or tungsten steel; and may also be a high strength organic material including PV or teflon; the material of the substrate can also be a glass plate, a ceramic plate or microcrystalline glass. More specifically, for example, by laser cutting, a metal plate with a certain width is selected, the thickness of the metal plate is consistent with the height of the support column 4, the metal plate is placed into a laser cutting machine, the travel is set to be circular, square or other set shapes, the metal plate is placed into a magnetic grinding device for polishing, the support column 4 is taken out for cleaning and drying, and finally the metal plate is placed into a storage tray of a support column 4 placement device for automatic placement. The support column 4 prepared and formed according to the process is smoother, and the quality of the vacuum glass is improved.
The glass pre-exhaust device 11 comprises an electron bombardment vacuum chamber and a heat radiation vacuum chamber, which respectively realize the surface treatment of the glass and the heating of the glass, and the positions of the two functional chambers can be interchanged. In the electron bombardment vacuum chamber, organic matters on the surface of the glass are removed through plasma to play a cleaning role, and meanwhile, high-speed electrons can collide with gas molecules physically adsorbed on the surface of the glass, so that the gas molecules also have a large amount of kinetic energy to be separated from the surface of the glass. In the heat radiation vacuum chamber, the temperature of the glass surface can be increased to accelerate the evaporation of moisture on the glass surface.
The vacuum bonding and sealing activation device 12 comprises a getter activation vacuum chamber, a sheet bonding vacuum chamber and a sealing vacuum chamber, wherein the getter is activated in the getter activation vacuum chamber, the glass substrate is bonded and aligned in the sheet bonding vacuum chamber, and then the glass substrate enters the sealing vacuum chamber for sealing.
Examples of the experiments
The vacuum glass production process of the scheme is subjected to parameter optimization research, the implementation mode is detailed in example 1, and the specific parameter settings are detailed in tables 1 and 2. In each of the tests 1 to 15, vacuum glasses having dimensions of 350mm × 350mm were prepared, and the first glass plate 1 and the second glass plate 2 each had a thickness of 5mm and a distance between the two glasses was 0.4 mm. In test 1, the step S5 was performed by first performing glass surface treatment and then heating the glass, and in test 2, the step S5 was performed by first performing glass heating and then performing glass surface treatment. Test 7 did not secure the solder 3 to the film layer. The selection of the parameters of runs 2-15 is consistent with run 1, except as described in tables 1 and 2 and in this example, run 1 was performed with reference to example 1. All test groups used cylindrical stainless steel support columns 4. The heat transfer coefficient (K value) of vacuum glass is measured according to the standard GB/T8484, which reflects the vacuum degree of the vacuum glass. To test the effect of the process parameters on the performance of the protocol, three replicates of each of trials 1-15 (three vacuum glasses were produced according to the experimental process and the K values were measured), the heat transfer coefficients (K values) in table 1 showing the average of the K values of the three trials, indicating a significant difference compared to trial 1 (t-test).
Table 1: parameter settings and Performance test results for experiments 1-6
Table 2: parameter settings and results of Performance tests of runs 7-15 (N/A means that this step was not performed, run 10 did not perform the entire S5 pre-venting step; run 11 did not perform the step of heating the first glass sheet 1 and the second glass sheet 2 to 50-200 ℃ in S5; run 12 did not perform the step of plasma-treating the first glass sheet 1 and the second glass sheet 2 in S5)
Tests 1-6 the vacuum glass prepared by the process of the scheme has an ideal heat transfer coefficient, the heat transfer coefficient can reflect the vacuum degree of the product, and a lower K value corresponds to a more ideal vacuum degree. In test 7, the solder 3 was not fixed to the film layer of the glass substrate in advance, the vacuum degree was poor, the produced vacuum glass was ordinary vacuum glass, and the K value was about 2.5. In S5 of test 8, the temperature at which the glass sheet was heated was too low, resulting in insufficient pre-evacuation and an excessively large K value of the vacuum glass obtained; in S5 of test 9, the temperature at which the glass sheet was heated was too high, and although the preliminary exhaust was sufficient, the energy consumption was too high. Test 10 did not involve preliminary evacuation, and the obtained vacuum glass had an excessively large K value. In S5 of test 11, the glass sheet was not heated, so that the preliminary evacuation was insufficient and the K value of the vacuum glass obtained was too large. In S5 of test 12, the preliminary exhaust was insufficient due to the plasma treatment not being performed, and the K value of the vacuum glass obtained was too large. In S7 of trial 13, the heat treatment temperature was too high, causing the sealed material to melt again and the vacuum to fail. In S7 of test 14, the heat treatment temperature was too low, and the degree of vacuum of the glass was not significantly affected. In S4 of test 15, the solder 3 was fixed to the film layer by laser welding, but the effect was not satisfactory, and the obtained vacuum glass had a high K value.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.