CN111257347A - Glass product detection method - Google Patents

Glass product detection method Download PDF

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Publication number
CN111257347A
CN111257347A CN201811458578.6A CN201811458578A CN111257347A CN 111257347 A CN111257347 A CN 111257347A CN 201811458578 A CN201811458578 A CN 201811458578A CN 111257347 A CN111257347 A CN 111257347A
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China
Prior art keywords
glass
glass piece
sample
piece
detected
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CN201811458578.6A
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CN111257347B (en
Inventor
马兰
陈梁
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Shanwei BYD Industrial Co Ltd
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Shanwei BYD Industrial Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
    • G01N21/958—Inspecting transparent materials or objects, e.g. windscreens
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/30—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces
    • G01B11/303—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces using photoelectric detection means

Abstract

The invention provides a detection method of a glass product. The method comprises the following steps: (1) carrying out surface detection on a sample to be detected, and selecting the sample to be detected with no visible gap on the surface to enter the step (2); (2) contacting the surface of the sample to be tested with an acidic reagent, and after the contacting, performing secondary surface detection on the sample to be tested, wherein the occurrence of a gap on the surface of the sample to be tested after the contacting is an indication that the sample to be tested is prepared by a low-temperature fusion process and the sample to be tested has a predetermined binding strength. By the method, the preparation method of the glass product can be conveniently and quickly determined, the bonding strength of the glass product can be basically judged, the application range of the glass product can be accurately judged, the glass product can be more reasonably and fully utilized, waste and improper use are avoided, and the economic benefit is improved.

Description

Glass product detection method
Technical Field
The invention relates to the technical field of glass product detection, in particular to a glass product detection method.
Background
At present, in order to expand the application range of glass and meet the use requirements of some specific fields, a plurality of glass pieces can be compounded together to form a glass product for use, so that the obtained compound glass product has the properties of glass and can also realize complex and fine shapes, but the currently obtained glass product is difficult to directly see the compounding process from the appearance and judge the use performance of the glass product, so that the glass product is limited to a certain extent when in use.
Thus, the related art of glass products still needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a glass product detection method.
The invention provides a glass product detection method. According to the embodiment of the invention, the method comprises the steps of (1) carrying out surface detection on a sample to be detected, and selecting the sample to be detected with no visible gap on the surface to enter the step (2); (2) contacting the surface of the sample to be tested with an acidic reagent, and after the contacting, performing secondary surface detection on the sample to be tested, wherein the occurrence of a gap on the surface of the sample to be tested after the contacting is an indication that the sample to be tested is prepared by a low-temperature fusion process and the sample to be tested has a predetermined binding strength. By the method, the preparation method of the glass product can be conveniently and quickly determined, the bonding strength of the glass product can be basically judged, the application range of the glass product can be accurately judged, the glass product can be more reasonably and fully utilized, waste and improper use are avoided, and the economic benefit is improved.
Drawings
Fig. 1 is a schematic flow diagram of a method of inspecting a glass article in one embodiment of the present invention.
Fig. 2A is a top view of a glass article in one embodiment of the invention.
Fig. 2B is a top view of a glass article according to another embodiment of the invention.
Fig. 2C is a top view of a glass article according to another embodiment of the invention.
Fig. 3A and 3B are schematic sectional views corresponding to a line a-a ' in fig. 2A, a line D-D ' in fig. 2B, and a line E-E ' in fig. 2C.
Fig. 4 is a schematic cross-sectional view of a glass article according to another embodiment of the present invention.
Fig. 5 is a schematic cross-sectional view of a glass article according to another embodiment of the invention.
Fig. 6 is a schematic plan view of a glass article according to another embodiment of the present invention.
Fig. 7 is a schematic sectional view taken along line D-D' in fig. 6.
FIG. 8 is a schematic plan view of a first and second frame-shaped glass pieces in accordance with one embodiment of the present invention.
Fig. 9 is a schematic structural view of a glass article according to another embodiment of the present invention, wherein the upper view is a schematic plan structural view, and the lower view is a schematic sectional structural view taken along line E-E' in the upper view.
Fig. 10 is a schematic structural view of a glass article according to another embodiment of the present invention, in which the upper view is a schematic plan structural view, and the lower view is a schematic sectional structural view taken along the line F-F' in the upper view.
Fig. 11 is a schematic plan view of a glass article according to another embodiment of the invention.
Fig. 12 is a schematic flow chart of a method of making a glass article according to one embodiment of the present invention.
Fig. 13 is a schematic flow chart of a method of making a glass article according to another embodiment of the present invention.
FIG. 14 is a schematic structural view of a glass article according to an embodiment of the present invention.
Fig. 15 is a schematic sectional view taken along line B-B' in fig. 14.
Fig. 16 is a schematic sectional view taken along line C-C' of fig. 15.
Fig. 17 is a schematic diagram of a binding force testing method in embodiment 1 of the present invention.
Fig. 18 is a photograph of a glass article of an embodiment of the present invention.
Fig. 19 is a photograph of a cut cross section of a glass article according to an embodiment of the present invention.
Fig. 20 is a photograph of the glass article in comparative example 1.
Fig. 21 is a photograph of a cut cross section of the glass article in comparative example 1.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The invention provides a glass product detection method. According to an embodiment of the present invention, referring to fig. 1, the method includes:
s100: and (5) carrying out surface detection on the sample to be detected, and selecting the sample to be detected with no visible gap on the surface to enter the step S200.
According to an embodiment of the present invention, in this step, the surface inspection may be visual observation or observation using a magnifying glass or a microscope. In some embodiments of the present invention, the surface of the glass article can be observed with a magnifying glass or microscope, and the specific magnification can be at least 100 times, at least 300 times, or at least 500 times, for example, 50 times, 100 times, 150 times, 200 times, 300 times, 350 times, 400 times, 450 times, or 500 times, and the like. In one specific example of the present invention, the surface of the sample to be measured has no gap visible to the naked eye at a magnification of 500 using a magnifying glass or microscope. Here, it should be noted that the visually observable slit refers to a slit having a smallest size which can be distinguished by naked eyes, and typically, the visually observable slit has a smallest size of 0.01 mm, and thus, the visually observable slit described herein refers to a slit having a width of not less than 0.01 mm. In the step, the performance of the sample to be detected is detected mainly by observing the appearance of the sample to be detected, if the sample to be detected has a gap which can be seen visually or observed through a magnifying glass or a microscope, the requirement that the sample to be detected cannot meet the appearance and the optical performance of electronic equipment is indicated, and meanwhile, the strength of a glass product to be detected is also indicated to be poor, so that the gap which can be seen by naked eyes can be seen if the sample to be detected is directly observed in the step, the use requirement is considered to be not met, and the sample to be detected with no gap which can be seen by naked eyes on the surface can enter the next detection step.
According to the embodiment of the invention, the sample to be detected can be a glass product formed by compounding two or more than two glass pieces, and whether a visible gap exists at the contact surface is mainly observed in the step, so that the sample to be detected can be effectively and quickly subjected to preliminary detection, and the efficiency is obviously improved.
According to the embodiment of the present invention, the material of the glass member used for forming the sample to be measured includes, but is not limited to, aluminosilicate (e.g., Corning glass, etc.), borosilicate (e.g., Schottky glass, etc.), cover glass (including high-alumina high-alkali aluminosilicate glass, soda-lime-silica glass, etc.), touch panel substrate glass (e.g., alkaline earth sodium pyroborate-aluminosilicate glass free of alkali and heavy metals (arsenic, antimony, barium), sodium glass, neutral borosilicate glass, etc.), display panel substrate glass (e.g., alkaline earth sodium pyroborate-aluminosilicate glass free of alkali and heavy metals (arsenic, antimony, barium), sodium glass, neutral borosilicate glass, etc.), TFT display panel substrate glass (e.g., alkaline earth sodium pyroborate-aluminosilicate glass brand glass free of alkali and heavy metals (arsenic, antimony, barium), etc.), the skilled person can make a flexible choice according to the actual need.
According to the embodiment of the invention, the specific structure and shape of the sample to be detected are not particularly limited, and the sample to be detected can be a flat plate structure, various complex 2.5-dimensional structures or 3-dimensional structures, so that the detection method can be used for detecting glass products with various structures and shapes, and the application range is wide.
The specific shape and structure of the glass article according to the embodiment of the present invention are not particularly limited, and those skilled in the art can flexibly select the shape according to the actual product requirements. The glass product is taken as an example of a shell formed by compounding a first glass piece and a second glass piece together: in some embodiments of the present invention, the first glass piece and the second glass piece may be specifically in a 2D structure, a 2.5D structure, or a 3D structure, and the surface of the first glass piece and the second glass piece that are in contact may be a plane, a curved surface (see fig. 4), or a combination of the plane and the curved surface, as long as the two are in contact without a gap, for example, if the surface of the first glass piece is an upward convex curved surface, the surface of the second glass piece is correspondingly an upward concave curved surface, and the specific shape and structure may be flexibly selected by those skilled in the art according to actual needs. Specifically, the first glass member and the second glass member may be each independently a plate glass member, a frame glass member (i.e., a closed ring glass member, such as a ring glass, a rectangular ring glass, or a ring glass having an outer periphery combined with a straight line and a curved line, etc.), or a strip glass (e.g., a long strip, a round strip, an irregular polygonal strip), and in some specific embodiments, referring to fig. 2A (rectangular ring glass) and 2B (circular ring glass), the first glass member is a plate glass, the second glass member is a frame glass, the frame glass member is combined on an outer periphery of the plate glass member (see fig. 3A), or the frame glass member is combined on an outer periphery of the plate glass member (see fig. 3B); in other embodiments, referring to fig. 2C, the first glass member is a plate glass, the second glass member is a strip glass, the strip glass is combined on the outer peripheral edge of the plate glass (specifically, the strip glass may be combined on the outer peripheral edge of one side, two sides, or more, and the cross-sectional structure of the outer peripheral edge of the two opposite sides is schematically shown in fig. 3A), or the frame glass is combined on the outer peripheral surface of the plate glass (specifically, the strip glass may be combined on the outer peripheral surface of one side, two sides, or more, and the cross-sectional structure of the outer peripheral surface of the two opposite sides is schematically shown in fig. 3B). Of course, the foregoing is merely illustrative of the structure of the glass article of the present invention and is not to be construed as limiting the invention.
According to some embodiments of the present invention, referring to fig. 5, the second glass piece 20 and the first glass piece 10 in the housing may form the following structure: the position where the first glass piece and the second glass piece are connected has an inner right-angle structure (a in figure 5); the position where the first glass piece and the second glass piece are connected has an inner step structure (b in figure 5); the outer surface of the position where the first glass piece and the second glass piece are connected is a curved surface (in fig. 5 c); the inner surface of the second glass piece is a curved surface (f in fig. 5) protruding outwards; the inner surface of the second glass piece is a slope (d in fig. 5) which gradually inclines inwards; the inner surface of the second glass piece is a slope (e in fig. 5) which gradually inclines outwards; the inner surface of the second glass member is a curved surface (g in fig. 5) convex inward.
According to other embodiments of the present invention, referring to fig. 6, the sample to be tested includes a first flat glass 11 and a second flat glass 21, wherein the second flat glass 21 has a rectangular, square, circular (see fig. 6 for a schematic structural diagram), polygonal or irregular shape. Specifically, a part of the surface of the first flat glass member 11 may contact with a part of the surface of the second flat glass member 21, and a part of the surface of the first flat glass member 11 may contact with a surface of the second flat glass member 21 (see fig. 6 and 7 for a schematic structural diagram), wherein a larger surface area of the first flat glass member 11 may be connected with a larger surface area of the second flat glass member 21. Of course, those skilled in the art will appreciate that other shapes and connections than those shown in the above figures are within the scope of the present application.
According to still further embodiments of the present invention, referring to fig. 8-11, the sample to be tested includes a first frame-shaped glass piece 12 and a second frame-shaped glass piece 22. Specifically, the shape of the first frame-shaped glass member and the second frame-shaped glass member is not particularly limited, and referring to fig. 8, the first frame-shaped glass member and the second frame-shaped glass member may be a circular ring, a square frame, a curved frame, or a frame shape combining a straight line and a curved line, and the like, and the connection position of the first frame-shaped glass member and the second frame-shaped glass member is also not particularly limited, and the first frame-shaped glass member and the second frame-shaped glass member may be vertically stacked (see fig. 9 and 10 for a structural schematic view), may be horizontally connected side by side (see fig. 11 for a structural schematic view), may be arranged in order (see fig. 9 and an upper view in fig. 11 for a structural.
Of course, those skilled in the art will appreciate that the shape and structure of the sample to be tested are only exemplary and should not be construed as limiting the present application, and the specific shape and structure of the sample to be tested can be flexibly selected according to the actual application requirements.
S200: contacting the surface of the sample to be tested with an acidic reagent, and after the contacting, performing secondary surface detection on the sample to be tested, wherein the occurrence of a gap on the surface of the sample to be tested after the contacting is an indication that the sample to be tested is prepared by a low-temperature fusion process and the sample to be tested has a predetermined binding strength.
According to the embodiment of the invention, the acidic solution used in the step is an acidic solution that can react with or corrode glass, if the sample to be tested is formed by compounding a plurality of glass pieces, if the compounding effect is not good, usually a gap can be seen through naked eyes or observation by using a magnifying glass or a microscope at the contact surface of two glass pieces, if the compounding effect is relatively good and the bonding strength between the glass pieces is relatively good, the contact surface of the two glass pieces is not distinguishable by naked eyes, but still has a certain difference with the glass piece body, after the research of the inventor, the corrosion speed of the contact surface of the two glass pieces by the acidic solution is faster than that of the glass piece body under the same conditions, and after the surface of the sample to be tested is contacted with the acidic solution, the corrosion speed of the contact surface of the two glass pieces is faster than that of the glass piece body, a gap may occur, and thus, after the sample to be measured is brought into contact with the acidic solution, the secondary surface inspection of the surface of the sample to be measured is performed, and if the secondary surface inspection is that a gap occurs on the surface of the sample to be measured, the sample to be measured on the surface is prepared by a low-temperature fusion process, and the sample to be measured has a predetermined bonding strength. The low-temperature fusion process means that the heating temperature does not exceed the softening point of the glass piece in the composite preparation process of the glass piece, and the preset bonding strength means the strength meeting the use requirement of the electronic equipment shell, so that the appearance performance, the optical performance and the mechanical performance of the glass product detected by the detection method can meet the use requirement of the electronic equipment shell, can be suitable for the electronic equipment shell, can realize a shell structure with a complex and fine structure, and even can realize a full-glass shell, meet the requirements of aesthetic sense and the like of users, and improve the user experience.
According to an embodiment of the present invention, taking a case where a sample to be tested includes a first glass piece and a second glass piece as an example, specific steps of the low-temperature fusion process described herein are described below, specifically, referring to fig. 12, the low-temperature fusion process may include:
s10: an activation treatment is performed on at least a portion of a surface of the first glass piece and at least a portion of a surface of the second glass piece, respectively, to form an activated surface.
According to an embodiment of the present invention, referring to fig. 13, before performing the activation treatment, the method may further include:
s11: and cleaning the surface to be activated of the first glass piece and the surface to be activated of the second glass piece. In some embodiments of the invention, the cleaning process may include: the glass piece is cleaned by acid detergent (such as hydrofluoric acid, sulfuric acid or peracetic acid), alkali detergent (such as sodium carbonate or calcium hypochlorite), organic reagent (such as acetone) and the like, and then dried. Therefore, the method is beneficial to removing oil stains and impurities on the surface of the glass piece and is beneficial to the implementation of the subsequent steps.
According to an embodiment of the invention, the activation treatment is adapted to form unsaturated chemical bonds on the surface of the first glass piece and the surface of the second glass piece. Therefore, the surface of the first glass piece or the second glass piece can generate unsaturated chemical bonds with high energy through activation treatment, and then when the first glass piece or the second glass piece is infinitely close to the second glass piece, the unsaturated chemical bonds on the surface of the glass pieces are combined with each other to form stable saturated chemical bonds, the internal uniformity of the obtained glass product is high, the bonding force between the first glass piece and the second glass piece is strong, so that the finally obtained glass product hardly influences light transmittance, and the use performance is good.
It should be noted that the description "unsaturated chemical bond" used herein refers to a chemical bond that contains unpaired electrons or lone pair electrons, has generally high energy, and cannot exist stably, for example, oxygen containing lone pair electrons is connected to a metal atom contained in a glass piece, specifically, the metal atom may be any metal atom contained in the glass, for example, including but not limited to an aluminum oxygen unsaturated bond, a sodium oxygen unsaturated bond, a potassium oxygen unsaturated bond, a calcium oxygen unsaturated bond, and the like; the nonmetal atoms in the glass piece can be connected with oxygen containing lone-pair electrons, and specifically, the nonmetal atoms can be any nonmetal atoms in the glass piece, such as but not limited to silicon-oxygen unsaturated bonds, boron-oxygen unsaturated bonds and the like; metal atoms or nonmetal atoms containing unpaired electrons or vacant orbitals (easy to form bonds with lone-pair electrons) can also be used, such as aluminum, sodium, potassium, calcium and the like containing unpaired electrons or vacant orbitals, and silicon dangling bonds, oxygen dangling bonds and the like can also be used; the "saturated chemical bond" refers to a chemical bond which does not contain unpaired electrons, has a low energy, and can exist stably, and specifically, the chemical bond may be formed after the above-mentioned unsaturated bonds are bonded to each other, and includes, but is not limited to, a silicon-oxygen-silicon bond, and the like.
According to an embodiment of the invention, the activation treatment is performed by a method of at least one of: a. treating with an activating solution, wherein the activating solution is acidic or alkaline; b. adopting plasma treatment; c. and (4) adopting ultraviolet light for treatment. For example, only the activation solution treatment, only the plasma treatment, or only the ultraviolet light treatment may be used, a combination of the activation solution treatment and the plasma treatment, a combination of the plasma treatment and the ultraviolet light treatment, a combination of the activation solution treatment and the ultraviolet light treatment, or the like may be used, or a combination of the activation solution treatment, the plasma treatment, and the ultraviolet light treatment may be used. Therefore, the method is simple and convenient to operate and easy to realize, the activated surfaces can be efficiently formed on the surfaces of the first glass piece and the second glass piece, the activating effect is better, and the binding force between the first glass piece and the second glass piece can be obviously improved.
When treated with an activation solution according to embodiments of the present invention, specific ways of activation treatment include, but are not limited to, dropping the activation solution onto the surfaces of the first and second glass pieces to be activated, or immersing the first and second glass pieces in the activation solution. When the plasma treatment is used, the first glass material and the second glass material may be placed in a plasma treatment apparatus, and plasma may be generated from an inert gas (e.g., a mixed gas of one or more of nitrogen, argon, and helium), a hydrogen-containing gas, or an oxygen-containing gas by means of discharge, high-frequency electromagnetic oscillation, shock wave, and high-energy radiation, to activate the surfaces of the first glass material and the second glass material. When the ultraviolet light is used for treatment, the ultraviolet light can be directly used for irradiating the first glass piece and the second glass piece, or the ultraviolet light can be used for irradiating the first glass piece and the second glass piece under the condition of the existence of ozone, so that the ozone can provide high-activity atomic oxygen to form volatile substances with free radicals generated after dirt is dissociated, and an active surface is generated.
According to an embodiment of the invention, the activation solution comprises: an acid (e.g., including but not limited to at least one of sulfuric acid, hydrochloric acid, hydrogen fluoride, ammonium bifluoride, nitric acid, and acetic acid) or a base (e.g., including but not limited to at least one of sodium carbonate, sodium bicarbonate, potassium hydroxide, sodium hydroxide, and aqueous ammonia); and an auxiliary agent including at least one of an oxidizing agent (such as at least one of potassium dichromate, hydrofluoric acid, hydrochloric acid, and hydrogen peroxide), an alcohol (for example, including, but not limited to, ethanol, methanol, and the like), an organic acid (for example, including, but not limited to, acetic acid, and the like), a sugar (for example, including, but not limited to, glucose, and the like), an amino acid, and a surfactant (for example, including, but not limited to, sodium dodecyl sulfate, and the like). Therefore, the activating solution can create a better acidic or alkaline environment, and unsaturated chemical bonds with higher energy can be formed on the surface of the glass piece, thereby being beneficial to the subsequent steps.
According to an embodiment of the invention, the activation solution is acidic or basic. Therefore, the activation treatment is simple and convenient to operate, easy to realize and good in activation effect. According to the embodiment of the present invention, when the activating solution is acidic, the activating solution further includes an oxidizing agent (e.g., potassium dichromate, potassium permanganate, nitric acid, hydrogen peroxide, etc.), whereby the activating ability of the activating solution can be improved, and unsaturated chemical bonds can be more easily formed on the surface of the glass member.
According to embodiments of the invention, the pH of the activation solution is no greater than 4 (e.g., 1, 2.5, 3, 3.5, 4, etc.), or the pH of the activation solution is 10-14 (e.g., 10, 10.5, 11, 11.5, 12, 12.5, 13, 13.5, 14, etc.). Therefore, the pH value of the activation solution can form more unsaturated chemical bonds within the range, and further the recombination between the first glass piece and the second glass piece is facilitated. If the acidity or alkalinity of the activating solution is too strong, the surface roughness of the glass piece is affected, so that the light transmittance of the glass product is relatively low; if the acidity or alkalinity of the activating solution is too weak, the activating effect on the surface of the glass member is relatively poor, and unsaturated chemical bonds are relatively less obtained.
In some embodiments of the invention, the starting materials for forming the activation solution include hydrogen peroxide and sulfuric acid. Therefore, the activating effect of the activating solution is better, more unsaturated chemical bonds are obtained, the first glass piece and the second glass piece are more favorably compounded, and the obtained glass product has almost no bubbles or fantasy colors. In some embodiments of the present invention, the activating solution is a mixture of hydrogen peroxide and sulfuric acid at a volume ratio of (1:3) - (3:7) (e.g., 1:3, 1:2.8, 1:2.6, 1:2.5, 1:2.3, etc.). Therefore, the activation solution has strong acidity or oxidizability, can promote the surface of the glass piece to be activated, generates more unsaturated chemical bonds, and has better activation effect. Compared with other proportioning ranges, the volume ratio of the hydrogen peroxide to the sulfuric acid is in the range, the activation effect is better, the light transmittance of the obtained glass product is higher, and the color illusion phenomenon is less.
In other embodiments of the present invention, the raw material forming the activation solution comprises potassium dichromate and sulfuric acid, for example, including but not limited to a mixture of potassium dichromate and sulfuric acid in a mass ratio of (1-3): 4 (e.g., 1:4, 1.5:4, 2:4, 2.5:4, 3:4, etc.). In still other embodiments of the present invention, the raw material forming the activation solution comprises hydrofluoric acid and ammonium bifluoride, for example, a mixed solution of hydrofluoric acid and ammonium bifluoride in a mass concentration of 5% to 40% (e.g., 5%, 10%, 15%, 20, 25%, 30%, 35%, 40%, etc.). Therefore, the surface of the glass piece can be activated, more unsaturated chemical bonds can be generated, and the activation effect is better.
In some embodiments of the invention, the starting materials for forming the activation solution include ammonia and hydrogen peroxide. In some embodiments of the present invention, the activating solution is a mixture of ammonia and hydrogen peroxide at a volume ratio of (1:1) - (1:5) (e.g., 1:1, 1:2, 1:3, 1:4, 1:5, etc.). Therefore, the oxidizing property of the activating solution is strong, the surface of the glass piece can be activated, more unsaturated chemical bonds can be generated, and the activating effect is better.
According to an embodiment of the present invention, the raw materials forming the alkaline activation solution include sodium hypochlorite and ammonia water. In some embodiments of the invention, the alkaline activation solution comprises a mixture of: 5 wt% -20 wt% of sodium hypochlorite, 5 wt% -30 wt% of ammonia water and 50 wt% -90 wt% of deionized water, wherein the content of the sodium hypochlorite can be 5 wt%, 10 wt%, 15 wt% or 20 wt%, the content of the ammonia water can be 5 wt%, 10 wt%, 15 wt%, 20 wt%, 25 wt% or 30 wt%, and the content of the deionized water can be 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, 75 wt%, 80 wt% or 90 wt%. Therefore, the activating solution can expose more unsaturated chemical bonds on the surface of the glass piece, and the activating effect is better. According to an embodiment of the present invention, the ultraviolet light treatment is performed by irradiating the surfaces of the first glass member and the second glass member with the ultraviolet light for 0.5 to 15 hours (e.g., 0.5 hour, 0.6 hour, 0.7 hour, 0.8 hour, 0.9 hour, 1.0 hour, 1.1 hour, 1.2 hour, 1.3 hour, 1.4 hour, 1.5 hour, 2 hour, 3 hour, 4 hour, 5 hour, 6 hour, 7 hour, 8 hour, 9 hour, 10 hour, 11 hour, 12 hour, 13 hour, 14 hour, 15 hour, etc.); or irradiating the surfaces of the first glass piece and the second glass piece with the ultraviolet light in the presence of ozone for 5 to 20 minutes (e.g., 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, etc.). Therefore, the surface of the glass piece can be promoted to generate and expose more unsaturated chemical bonds, and the activation effect is better.
According to an embodiment of the present invention, the plasma treatment is performed by using O under the excitation frequency of 10MHz-15MHz (such as 10.25MHz, 10.5MHz, 11MHz, 11.25MHz, 11.5MHz, 11.75MHz, 12MHz, 13MHz, 13.8MHz, 14MHz, 14.5MHz, 15MHz, etc.)2Plasma and N2/H2Treating the surface of the first glass piece and the second glass piece with at least one of plasma for 10-30 minutes (e.g., 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, 21 minutes, 2 minutes)2 minutes, 23 minutes, 4 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes, or 30 minutes). Therefore, the surface of the glass piece can be promoted to generate and expose more unsaturated chemical bonds, and the activation effect is better.
Wherein, it is to be noted that, the description mode "N" adopted in the present text2/H2Plasma "means N2And H2The activation treatment may be O alone2Plasma process, using N alone2/H2Plasma treatment or simultaneous use of O2Plasma and N2/H2The plasma is performed.
According to an embodiment of the present invention, the activation treatment is performed at room temperature-200 degrees celsius, for example, the activation treatment may be performed at 25 degrees celsius, 40 degrees celsius, 50 degrees celsius, 60 degrees celsius, 70 degrees celsius, 80 degrees celsius, 90 degrees celsius, 100 degrees celsius, 110 degrees celsius, 130 degrees celsius, 150 degrees celsius, 170 degrees celsius, 190 degrees celsius, 200 degrees celsius, or the like. Therefore, the activation treatment in the temperature range is more beneficial to promoting more unsaturated chemical bonds to form, and the activation effect is better. Compared with the temperature range, if the temperature of the activation treatment is too high, the activation solution is volatile, the service life is relatively short, and the activation effect is relatively poor; if the temperature of the activation treatment is too low, the glass activation effect is relatively poor.
According to the embodiment of the present invention, since the unsaturated chemical bonds formed after the activation treatment are extremely reactive, and are easily reacted by contacting with oxygen in the air, the residence time is short, the first glass member and the second glass member are placed in a vacuum environment for a time after the activation treatment until the contact is completed. Therefore, unsaturated chemical bonds formed after the activation treatment are not contacted with oxygen in the air to react, the retention time of the unsaturated chemical bonds is prolonged, and the subsequent steps are facilitated, so that the first glass piece and the second glass piece have preset bonding strength. In some embodiments of the present invention, the activation process may be performed directly in a vacuum environment, or the first glass piece and the second glass piece may be placed in a vacuum environment after the activation process and then maintained until the contact is completed. Thereby, the reactivity of the unsaturated chemical bond can be maintained as much as possible, so that the first glass member and the second glass member have a predetermined bonding strength therebetween.
According to an embodiment of the present invention, the activated surface obtained after the activation treatment has a small water droplet angle, such as not more than 10 degrees, for example, 1 degree, 2 degrees, 3 degrees, 4 degrees, 5 degrees, 6 degrees, 7 degrees, 8 degrees, 9 degrees, 10 degrees, etc. This indicates that the activated surface forms more unsaturated bonds with higher energy, which facilitates bonding of the first glass piece and the second glass piece with a predetermined bonding strength. According to embodiments of the present invention, the first glass piece and the second glass piece have a surface Roughness (RA) of no greater than 0.2 microns, such as 0.2 microns, 0.18 microns, 0.16 microns, 0.15 microns, 0.12 microns, 0.1 microns, 0.08 microns, 0.05 microns, and the like. Thereby, it is more advantageous to obtain a predetermined bonding strength. In other embodiments of the present invention, the first and second glass pieces have a surface roughness of no greater than 0.2 microns and an activated surface water drop angle of no greater than 10 degrees after activation.
S20: the activated surface of the first glass piece is brought into contact with the activated surface of the second glass piece to form the sample to be tested (otherwise known as a glass article).
According to an embodiment of the invention, the contacting causes bonds between unsaturated chemical bonds on the activated surface of the first piece of glass and unsaturated chemical bonds on the activated surface of the second piece of glass to form stably existing saturated chemical bonds. Therefore, a new saturated chemical bond is formed at the contact position, and the predetermined bonding strength is ensured between the first glass piece and the second glass piece, so that the internal uniformity of the glass product is improved, and the optical performance of the glass product is improved.
According to an embodiment of the invention, the contacting is performed in a vacuum environment. Therefore, the activated unsaturated chemical bond can not be contacted with oxygen in the air to react, the retention time of the unsaturated chemical bond is prolonged, and the subsequent steps can be favorably carried out. It should be noted that, because the unsaturated chemical bond formed after the activation treatment has extremely high activity, it is very easy to contact with oxygen in the air to react, and the residence time is short, and the contact under vacuum environment can avoid the unsaturated chemical bond from contacting with air to react, so that it keeps high activity, and effectively makes the predetermined bonding strength between the first glass piece and the second glass piece.
According to the embodiment of the invention, the contact can be carried out under the heating condition, the first glass piece and the second glass piece are required to be heated, in some embodiments of the invention, the heating area can be consistent with the area of the first glass piece and can also be consistent with the area of the second glass piece, in some specific embodiments of the invention, the second glass piece is heated at the position where the second glass piece is overlapped with the first glass piece, therefore, the first glass piece and the second glass piece can be fixed together by effective heating, meanwhile, the heat utilization rate is high, the energy consumption is saved, and the influence of heating on the glass pieces of other parts can be reduced as much as possible.
According to an embodiment of the invention, the contacting is performed at a first predetermined temperature, the first predetermined temperature not exceeding a softening point of the first and second glass pieces. Therefore, the phenomena of surface scalding, distortion and unevenness caused by overhigh temperature hardly occur, the light transmittance of the finally obtained glass product is hardly influenced, and the appearance is attractive, so that a proportional product obtained by the method can hardly be distinguished from other glass products without a certain detection method.
It should be noted that, since the softening point of the glass member means the temperature at which the glass member starts to soften, and the description "the first predetermined temperature does not exceed the softening point of the first glass member and the second glass member" as used herein means that the first predetermined temperature does not exceed the lower temperature of the softening points of the first glass member and the second glass member.
In some embodiments of the present invention, the first predetermined temperature is between 200 ℃ and 900 ℃, such as 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, and the like. Therefore, the first preset temperature does not exceed the softening point of the glass piece, the outer surface of the glass is not scalded due to low temperature, the glass is not softened, and the surface of the glass is not deformed and uneven, so that the light transmittance of the finally obtained glass product is improved, and the appearance of the glass product is attractive and attractive. If the first preset temperature is too high, the glass pieces are easy to soften, the outer surface of the glass pieces can cause scald deformation, the surface is uneven, and new saturated chemical bonds are not formed between the two glass pieces, so that the optical performance of the glass product is influenced; if the first predetermined temperature is too low, the bond strength between the glass pieces is low and the resulting glass article has low strength. In some embodiments of the present invention, the first predetermined temperature is between 250-750 ℃, such as 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, and the like. Therefore, the glass product is more beneficial to compounding the first glass piece and the second glass piece, the preset bonding strength is obtained, the phenomenon of surface distortion and unevenness caused by overhigh temperature is hardly caused, the finally obtained glass product has higher light transmittance, and the appearance is more attractive and attractive.
According to an embodiment of the invention, the contacting is performed under pressurized conditions. Therefore, the first glass piece and the second glass piece are more favorably welded together under the pressurizing condition, a glass product with better strength is formed, and bubbles or fantasy colors are easily generated in the glass product. In some embodiments of the invention, the pressurization is at a pressure of 0.05 to 10MPa, such as 0.1MPa, 0.5MPa, 1.0MPa, 1.5MPa, 2.0MPa, 3.0MPa, 5.0MPa, 7.0MPa, 9.0MPa, and the like. Therefore, the first glass piece and the second glass piece have better composite effect, and the strength of the glass product is proper. If the pressure is too high, the surface of the glass is easy to have indentation, the glass structure is easy to deform, if the pressure is too low, the bonding force between the glass pieces is relatively low, and bubbles and fantasy colors are easy to appear in the glass product.
According to the embodiment of the invention, in the pressurizing process, the pressurizing treatment is carried out at the position where the second glass piece is overlapped with the first glass piece, so that the composite strength of the first glass piece and the second glass piece can be ensured, the defects of bending, deformation and the like of other parts of the first glass piece and the second glass piece caused by the pressurizing treatment can be avoided, the pressure bearing area is small, the pressure intensity can be large, the large bonding strength can be realized under the small pressure condition, and the reduction of bubbles and fantasy colors is facilitated.
In some embodiments of the present invention, the glass article may be prepared by:
firstly, cleaning a first glass piece and a second glass piece by using a detergent, removing oil stains and impurities, and drying;
and secondly, putting the cleaned first glass piece and the cleaned second glass piece into an activating solution for activating treatment, heating for a period of time at room temperature of 200 ℃ below zero, naturally cooling, washing the residual solution on the surface by pure water, drying, and activating the surfaces of the first glass piece and the second glass piece. The activation mainly aims at increasing unsaturated chemical bonds on the surface of the glass piece, and the unsaturated chemical bonds on the surface of the glass piece are combined to form new stably existing saturated chemical bonds during compounding so as to promote the subsequent compounding process;
third, the activated surface of the first glass piece and the activated surface of the second glass piece are contacted and heated to a temperature below the softening point of the glass while applying pressure to bond at least a portion of the surfaces of the first and second glass pieces together to form the glass article.
The inventor finds that the method is simple and convenient to operate and easy to realize, a new saturated chemical bond is formed between the first glass piece and the second glass piece after activation treatment, the binding force is strong, the strength of the formed glass product is good, the uniformity of the interior of the glass product is high, the surface of the glass product is smooth, the appearance is attractive and attractive, the optical performance is hardly influenced, and the light transmittance is high. Of course, those skilled in the art will appreciate that the low temperature fusion process described above is merely illustrative and should not be construed as limiting the present invention, and that other glass articles formed by the low temperature fusion process can be detected by the detection method of the present invention.
According to an embodiment of the present invention, the transmittance of the glass product obtained by the low-temperature fusion process is not lower than 95% of the transmittance of the lower transmittance glass piece of the first glass piece and the second glass piece, for example, the transmittance of the glass product is not lower than 95%, 96%, 97%, 98%, 99%, 100%, etc. of the transmittance of the lower transmittance glass piece of the first glass piece and the second glass piece. Specifically, if the light transmittance of the first glass member is greater than that of the second glass member, the light transmittance of the glass article is not less than 95% of that of the second glass member, and if the light transmittance of the first glass member is less than that of the second glass member, the light transmittance of the glass article is not less than 95% of that of the first glass member. Therefore, the glass product has high light transmittance and good optical performance, almost has no bubbles or fantasy colors, can realize various complex and fine shapes and structures such as but not limited to a special-shaped structure, a six-sided ring-wrapped structure and the like by connecting the first glass piece and the second glass piece, and cannot distinguish the glass product prepared by the method from the glass product prepared by other processes if the glass product has the optical properties such as no specific detection method.
It should be noted that the light transmittance of the glass member is generally related to the thickness of the glass member, and when the thickness is not greatly different and the influence of the thickness on the light transmittance is not significant, the "light transmittance of the glass article is not lower than 95% of the lower light transmittance glass member of the first and second glass members" described in the present invention can neglect the influence of the thickness on the glass member and the glass article, for example, the light transmittance at the position where the first and second glass members are stacked in the glass article is not lower than 95% of the lower light transmittance glass member of the first and second glass members, and if the thickness of the first or second glass member is large and the influence of the thickness on the light transmittance is significant, "the light transmittance of the glass article is not lower than 95% of the lower light transmittance glass member of the first and second glass members" described in the present invention can be not lower than the light transmittance at the position where the first and second glass members are stacked in the glass article and the above-mentioned thickness are not lower than the light transmittance The stack locations have the same or approximately the same thickness of 95% of the lower transmittance glass pieces of the first and second glass pieces.
According to the embodiment of the invention, the acidic solution can be hydrofluoric acid solution due to better reaction, faster speed and higher detection efficiency. Therefore, hydrofluoric acid can easily react with glass, and can effectively distinguish the positions of the glass piece body and the contact surface, so that the composite position can be accurately detected, and better guidance can be provided for reasonably utilizing a sample to be detected. According to an embodiment of the present invention, the acidic solution is a 5-40% by mass hydrofluoric acid solution, such as 5%, 10%, 15%, 20%, 25%, 30%, 35% or 40% by mass hydrofluoric acid solution, etc. Therefore, the raw materials are wide in source and easy to obtain, the cost is low, and the operation safety is high while the good detection effect is ensured.
According to the embodiment of the invention, the sample to be tested is contacted with hydrofluoric acid solution with mass concentration of 5% -40% for 30 seconds to 20 minutes (such as 30 seconds, 1 minute, 5 minutes, 10 minutes, 15 minutes, 20 minutes and the like), the surface of the sample to be tested has a width of 0.1-300 micrometers (such as 0.1 micrometer, 5 micrometer, 10 micrometer, 15 micrometer, 20 micrometer, 25 micrometer, 30 micrometer, 35 micrometer, 40 micrometer, 45 micrometer, 50 micrometer, 55 micrometer, 60 micrometer, 65 micrometer, 70 micrometer, 75 micrometer, 80 micrometer, 85 micrometer, 90 micrometer, 95 micrometer, 100 micrometer, 105 micrometer, 110 micrometer, 115 micrometer, 120 micrometer, 125 micrometer, 130 micrometer, 135 micrometer, 140 micrometer, 145 micrometer, 150 micrometer, 155 micrometer, 160 micrometer, 165 micrometer, 170 micrometer, 175 micrometer, 180 micrometer, 185 micrometer, 190 micrometer, 195 micrometer, 200 micrometer, 100 micrometer, 205 microns, 210 microns, 215 microns, 220 microns, 225 microns, 230 microns, 235 microns, 240 microns, 245 microns, 250 microns, 255 microns, 260 microns, 265 microns, 270 microns, 275 microns, 280 microns, 285 microns, 290 microns, 295 microns, 300 microns, etc.) is an indication that the sample under test was prepared for a low temperature fusion process and that the sample under test has a predetermined binding strength. Therefore, the synthesis method and the bonding strength of the sample to be detected can be accurately detected, and the detected sample to be detected can meet the use requirement of the electronic equipment.
According to some embodiments of the invention, any one of the following (a) to (h) is an indication that the sample to be tested is prepared for a low temperature fusion process and that the sample to be tested has a predetermined binding strength: (a) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 5% for 300 seconds, wherein the width of the gap is 0.1-30 microns; (b) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 10% for 300 seconds, wherein the gap with the width of 0.5-50 micrometers (such as 0.5 micrometer, 1 micrometer, 5 micrometer, 10 micrometer, 20 micrometer, 30 micrometer, 40 micrometer or 50 micrometer) appears on the surface of the sample to be detected; (c) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 20% for 300 seconds, wherein the gap with the width of 0.5-100 micrometers (such as 0.5 micrometer, 1 micrometer, 5 micrometer, 10 micrometer, 20 micrometer, 30 micrometer, 40 micrometer, 50 micrometer, 60 micrometer, 70 micrometer, 80 micrometer, 90 micrometer or 100 micrometer) appears on the surface of the sample to be detected; (d) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 40% for 300 seconds, wherein the gap with the width of 2-100 micrometers (such as 2 micrometers, 5 micrometers, 10 micrometers, 20 micrometers, 30 micrometers, 40 micrometers, 50 micrometers, 60 micrometers, 70 micrometers, 80 micrometers, 90 micrometers or 100 micrometers) appears on the surface of the sample to be detected; (e) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 5% for 600 seconds, wherein the gap with the width of 1-50 micrometers (such as 1 micrometer, 5 micrometers, 10 micrometers, 20 micrometers, 30 micrometers, 40 micrometers or 50 micrometers) appears on the surface of the sample to be detected; (f) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 10% for 600 seconds, wherein the gap with the width of 1-80 micrometers (such as 10 micrometers, 20 micrometers, 30 micrometers, 40 micrometers, 50 micrometers, 60 micrometers, 70 micrometers or 80 micrometers) appears on the surface of the sample to be detected; (g) contacting the sample to be detected with hydrofluoric acid with a mass concentration of 20% for 600 seconds, wherein the gap with a width of 3-120 micrometers (such as 3 micrometers, 5 micrometers, 10 micrometers, 20 micrometers, 30 micrometers, 40 micrometers, 50 micrometers, 60 micrometers, 70 micrometers, 80 micrometers, 90 micrometers, 100 micrometers, 110 micrometers or 120 micrometers) appears on the surface of the sample to be detected; (h) and contacting the sample to be detected with hydrofluoric acid with the mass concentration of 40% for 600 seconds, wherein the gap with the width of 5-120 micrometers (such as 5 micrometers, 10 micrometers, 20 micrometers, 30 micrometers, 40 micrometers, 50 micrometers, 60 micrometers, 70 micrometers, 80 micrometers, 90 micrometers, 100 micrometers, 110 micrometers or 120 micrometers) appears on the surface of the sample to be detected. Therefore, the detection result is accurate, and the performance requirement of the electronic equipment shell can be met through the detected sample to be detected.
In the examples of the present invention, the width of the gap is given according to the glass material, experimental conditions and test conditions specifically used by the inventor, and the width varies from one glass material to another, from one experimental condition to another or from one test condition to another.
According to embodiments of the present invention, the sample to be tested may be a glass article formed by combining a plurality of glass pieces together, as described above. In some embodiments of the present invention, the sample to be tested comprises a first glass member and a second glass member connected at least partially on their surfaces, the contact position of the first glass member and the second glass member defining a contact surface, and after contacting the sample to be tested with the acidic solution, a gap appears on the surface of the sample to be tested and extends along the contact surface, which is indicative of the sample to be tested being prepared for a low temperature fusion process and the sample to be tested having a predetermined bonding strength. Therefore, the detection result is accurate and credible, and the method has very important practical guiding significance for application of the glass product.
According to the embodiment of the invention, the surface of the sample to be detected, which is subjected to surface detection or contacted with the acidic solution in the detection process, can be the outer surface of the sample to be detected directly or can be a surface formed by properly processing the sample to be detected. Specifically, the detection method may include: (1-1) cutting the sample to be detected in a direction forming a preset angle with the contact surface to obtain a cut surface; (1-2) carrying out surface detection on the cut surface, and selecting the sample to be detected with no visible gap on the surface to enter the step (1-3); (1-3) contacting the cut surface with an acidic reagent and performing the secondary surface inspection on the cut surface after the contacting, wherein after the contacting, the appearance of a gap in the surface of the cut surface and the extension of the gap along the contact surface are indicative that the sample to be tested is prepared for a low temperature fusion process and the sample to be tested has a predetermined bond strength. The preset angle is not particularly limited, and the contact surface can be observed in a wider range as long as the cutting surface is intersected with the contact surface, the condition inside the contact surface can be observed, the combination condition of the contact surface can be determined more comprehensively and accurately by observing the cutting surface, and the detection result is more accurate and reliable.
According to a specific example of the present invention, referring to fig. 14, fig. 15 and fig. 16, a case where a sample to be measured includes a first glass member 1 and a second glass member 2 connected to each other at partial surfaces is described in detail, specifically, a cross section taken along a direction perpendicular to a contact surface where the first glass member 1 and the second glass member 2 are connected is defined as a first cross section (see fig. 15 for a schematic structural diagram), and a gap 3 appears at the contact surface after the first cross section is contacted with hydrofluoric acid (see fig. 16 for a schematic structural diagram, and a shape of the gap shown in fig. 16 is merely an exemplary illustration and is not to be construed as a limitation to the present application, and according to a hydrofluoric acid etching process, a person skilled in the art can understand that a specific gap shape can be various geometric shapes or irregular random shapes). Specifically, the first cross section obtained after cutting the glass product is obtained (for more convenient observation, the first cross section obtained after cutting can be polished to remove burrs, and the observation effect is better), no gap is formed by visual or microscopic magnification of 500 times, when the first cross section is corroded in hydrofluoric acid solution with mass concentration of 5% -40% for 30 seconds to 20 minutes, the composite surface of the first glass piece and the second glass piece is corroded to form a gap, the width W of the gap can be 0.1-300 micrometers, such as 0.1 micrometer, 5 micrometer, 10 micrometer, 15 micrometer, 20 micrometer, 25 micrometer, 30 micrometer, 35 micrometer, 40 micrometer, 45 micrometer, 50 micrometer, 55 micrometer, 60 micrometer, 65 micrometer, 70 micrometer, 75 micrometer, 80 micrometer, 85 micrometer, 90 micrometer, 95 micrometer, 100 micrometer, 105 micrometer, 110 micrometer, 115 micrometer, 120 micrometer, 125 micrometer, 130 micrometer, stainless steel, stainless, 135 microns, 140 microns, 145 microns, 150 microns, 155 microns, 160 microns, 165 microns, 170 microns, 175 microns, 180 microns, 185 microns, 190 microns, 195 microns, 200 microns, 205 microns, 210 microns, 215 microns, 220 microns, 225 microns, 230 microns, 235 microns, 240 microns, 245 microns, 250 microns, 255 microns, 260 microns, 265 microns, 270 microns, 275 microns, 280 microns, 285 microns, 290 microns, 295 microns, 300 microns, and the like. Therefore, the sample to be detected can be prepared by the low-temperature fusion process, has preset bonding strength, and can meet the use requirement of the electronic equipment shell.
The inventor finds that the preparation method of the glass product can be conveniently and quickly determined by the method, the bonding strength of the glass product can be basically judged, the application range of the glass product can be accurately judged, the glass product can be more reasonably and fully utilized, waste and improper use are avoided, and the economic benefit is improved.
According to the embodiment of the invention, the glass product detected by the detection method can be effectively applied to electronic equipment shells, such as shells of mobile phones and tablet computers, and the like, and can also be a protective cover plate, a rear shell, a color film substrate or a substrate in an array substrate of a display device, and the detection method can be specifically selected according to actual conditions.
The following describes in detail embodiments of the present application, and the structures of samples to be tested related to the embodiments described below are all shown in fig. 14.
Example 1
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe glass product is cut in the thickness direction at the joint position where the first glass piece and the second glass piece are connected to form a section (see fig. 15), the section is polished to make no visible gap (or composite trace) by visual observation or microscope magnification of 500 times (see fig. 19), and then the section is contacted with hydrofluoric acid solution with the mass concentration of 10% for 5 minutes, the contact surface of the first glass piece and the second glass piece is corroded to form a visible gap, and the gap width is about 10 microns.
The preparation method of the glass product in the embodiment comprises the following steps:
cleaning a first glass piece and a second glass piece (the first glass piece and the second glass piece are made of Corning GG3 glass (the visible light transmittance is 91% -93%) with the thickness of 0.7 mm) by using a mixed solution of hydrofluoric acid, sulfuric acid and surfactant sodium dodecyl sulfate, removing oil contamination impurities, drying, putting a mixed solution of hydrogen peroxide and sulfuric acid (1:3) into the dried glass pieces, heating for 1 hour at 80 ℃, naturally cooling, cleaning the residual solution on the surface by pure water, drying, activating the surface of the glass piece, and enabling the contact angle of the surface of the activated glass piece to be less than 10 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 650 ℃, simultaneously applying pressure of 0.4MPa, maintaining the temperature and the pressure for 3 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% to visible light (wave band 380 nm-720 nm), and the bonding strength of the glass product is tested, wherein a test sample is schematically shown in fig. 14 (wherein, the length L of each of the glass pieces 1 and 2 is 24mm, the width W1 is 12mm, and the length L1 of the overlapping area of the two glass pieces is 6mm), and a test method is schematically shown in fig. 17, and specifically, the glass product is stretched at a speed of 5 mm/min by using a universal testing machine until the glass is broken. The test results are: the bonding strength (150N) between the first glass piece or the second glass piece is not lower than the drawing strength when the glass piece is broken before compounding, which indicates that the two pieces of glass are compounded together, and the bonding strength meets the use requirement of the electronic equipment.
Example 2
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe combination position has no obvious bubbles and magic colors, the combination position of the first glass piece and the second glass piece in the glass product is cut along the thickness direction to form a section, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the combination effect is good, when the section is corroded in 10% hydrofluoric acid solution for 5 minutes, the combination surface of the first glass piece and the second glass piece is corroded, and gaps and seams can be seen by naked eyesThe gap width is 1-10 microns.
In this embodiment, the first glass member and the second glass member are made of corning GG5 glass (with a visible light transmittance of 91% to 93%) with a thickness of 1 mm.
A method of compositing a first glass piece (a sheet glass piece) and a second glass piece (a donut-shaped frame glass piece) comprising:
firstly, K is put in2Cr2O760g of the solution was dissolved in 270g of water, 44ml of concentrated sulfuric acid was slowly added, and the first glass piece and the second glass piece were soaked with the resulting mixed acid solution (2 hours at room temperature or 30 minutes at 50 ℃). After being taken out, the chromium ions remained on the surface are washed away by 10 percent nitric acid washing liquor. And cleaning for 10 minutes by pure water, and then drying by blowing, so that the surface of the glass piece is activated. The surface roughness of the glass piece surface before activation was 0.612 nm. And (3) laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 750 ℃, simultaneously applying 2MPa of pressure, maintaining the temperature and the pressure for 5 hours, and slowly cooling to compound the glass partially or completely to obtain a glass composite (a structural schematic diagram is shown in figure 2B).
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is more than or equal to 91%, and the optical performance and the service performance are better. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged at a tensile force of 155 newtons (i.e., 2.15MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 3:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which indicates that the composite effect is good, and when the section is corroded in 5 mass percent hydrofluoric acid solution for 5 minutes, the first glass piece is corroded for 5 minutesThe composite surface of the glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.5-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece (sheet glass piece) and a second glass piece (strip glass piece) comprises:
firstly, K is put in2Cr2O720g was dissolved in 270g of water, 44ml of concentrated sulfuric acid was slowly added, and the first glass piece and the second glass piece were soaked with the resulting mixed acid solution (6 hours at room temperature or 150 minutes at 50 ℃). After being taken out, the chromium ions remained on the surface are washed away by 10 percent nitric acid washing liquor. And cleaning for 10 minutes by pure water, and then drying by blowing, so that the surface of the glass piece is activated. The surface roughness of the glass piece surface before activation was 0.592 nm. And (3) laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 700 ℃, simultaneously applying 1MPa of pressure, maintaining the temperature and the pressure for 4 hours, and slowly cooling to compound the glass partially or completely to obtain the glass product (the structural schematic diagram is shown in figure 2C).
The obtained glass product has the light transmittance of more than or equal to 91 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and use performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged under a tensile force of 160 newtons (i.e., 2.22MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 4:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe compounding position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no compounding trace can be seen by visual observation or microscope magnification of 500 times, which shows that the compounding effect is good, and the section is subjected to hydrogen with the mass concentration of 10 percentWhen the first glass piece and the second glass piece are corroded in the hydrofluoric acid solution for 5 minutes, a gap can be seen by naked eyes, and the width of the gap is 10-50 micrometers.
In this embodiment, the first glass member and the second glass member are made of corning GG3 glass (with a visible light transmittance of 91% to 93%) with a thickness of 0.7 mm.
A method of compositing a first glass piece (a sheet glass piece) with a second glass piece (a rectangular frame-shaped glass piece) comprises:
firstly, at room temperature, the first glass piece and the second glass piece are sequentially put into acetone, peroxyacetic acid solution or calcium hypochlorite solution for cleaning for 30 minutes respectively, then taken out, washed by pure water and dried. And (3) putting the cleaned first glass piece and the second glass piece into a mixed solution of ammonia water and hydrogen peroxide (1:2), treating for 50 minutes at 40 ℃, cleaning the residual solution on the surface for 10 minutes by pure water, and drying to dry, so that the surface of the glass piece is activated. The first glass piece and the second glass piece are contacted with each other, the first glass piece and the second glass piece are heated to 700 ℃, the pressure of 0.5MPa is applied, the temperature and the pressure are maintained for 2 hours, and then the glass is partially or completely compounded together to obtain the glass product, wherein the structural schematic diagram is shown in figure 2A.
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is 92%, and the optical performance and the service performance are better. The surface of the glass product is flat and smooth, and the composite position has no defects such as bubbles, impurity points, magic colors and the like which are visible to the naked eye. The bonding strength was measured according to the method of example 1, and the results showed that the bonding strength was 151 n (i.e., 2.1MPa), no change was observed at the bonding position, and the glass pieces broke, indicating that the two pieces of glass had fused together.
Example 5
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed by cutting along the thickness direction at the joint position where the first glass piece and the second glass piece are connected in the obtained glass product, and the section is polished, visually observed or microscopically observedWhen the section is corroded in a hydrofluoric acid solution with the mass concentration of 40% for 2 minutes, obvious gaps can be formed on the composite surface on the section by naked eyes.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% -93%).
A method of compositing a first glass piece (a sheet glass piece) with a second glass piece (a donut-shaped frame glass piece) comprises:
firstly, at room temperature, the first glass piece and the second glass piece are sequentially put into acetone, peroxyacetic acid solution or calcium hypochlorite solution for cleaning for 30 minutes respectively, then taken out, washed by pure water and dried. And (3) putting the cleaned first glass piece and the second glass piece into a mixed solution of ammonia water and hydrogen peroxide (1:3), treating for 40 minutes at 40 ℃, cleaning the residual solution on the surface for 10 minutes by pure water, and drying to dry, so that the surface of the glass piece is activated. And (3) contacting the first glass piece and the second glass piece which are subjected to surface activation, heating to 610 ℃, simultaneously applying 1MPa of pressure, maintaining the temperature and the pressure for 2 hours, and slowly cooling to compound the glass partially or completely to obtain the glass product, wherein the structural schematic diagram is shown in fig. 2B.
In the above embodiment, the obtained glass product has a visible light transmittance of 91%, and thus has good optical properties and usability. The composite position of the first glass piece and the second glass piece has no obvious defects of bubbles, magic colors and the like. The bonding strength was tested according to the test method in composite example 1, and the test results were: the bond position did not change under a pull of 159 newtons (i.e., 2.21MPa), and either the first glass piece or the second glass piece broke, indicating that the two pieces of glass had fused together.
Example 5
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe recombination position has no obvious bubbles and fantasy colors, and the obtained glass product has thickness along the joint position where the first glass piece and the second glass piece are connectedAnd cutting the section in the direction to form a section, polishing the section, and observing the section by visual observation or microscope magnification of 500 times to obtain a good composite effect, wherein when the section is corroded in a hydrofluoric acid solution with the mass concentration of 20% for 5 minutes, a clear gap is formed on the composite surface on the section by naked eyes, and the width of the gap is 0.5-20 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% -93%).
A method of compositing a first glass piece (sheet glass piece) with a second glass piece (strip glass piece) comprises:
firstly, at room temperature, the first glass piece and the second glass piece are sequentially put into acetone, peroxyacetic acid solution or calcium hypochlorite solution for cleaning for 30 minutes respectively, then taken out, washed by pure water and dried. And (3) putting the cleaned first glass piece and the second glass piece into a mixed solution of sodium hypochlorite and ammonia water (the mass fractions of sodium hypochlorite, ammonia water and deionized water are 10%, 30% and 60%), treating for 60 minutes at room temperature, cleaning the surface with pure water for 10 minutes, drying the surface, and activating the surface of the glass piece. And (3) contacting the first glass piece and the second glass piece which are subjected to surface activation, heating to 450 ℃, simultaneously applying 1.5MPa of pressure, maintaining the temperature and the pressure for 5 hours, and slowly cooling to compound the glass partially or completely together to obtain the glass product, wherein the structural schematic diagram is shown in fig. 2C.
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is 91.5%, and the optical performance and the service performance are better. The bonding strength was tested according to the test method in example 1, and the test results were: the bonding position was unchanged at a tensile force of 155 newtons (i.e., 2.15MPa), and the first glass piece or the second glass piece broke, indicating that the two pieces of glass had fused together.
Example 6
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAt the composite position, without obvious bubbles and fantasy colors, the obtained glassThe glass product is characterized in that a section is formed by cutting along the thickness direction at the joint position where the first glass piece and the second glass piece are connected in the glass product, the section is polished, and no composite trace can be seen visually or under the magnification of 500 times by a microscope, so that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 15% for 5 minutes, obvious gaps can be formed at the composite surface on the section by naked eyes.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% -93%). The first glass piece is in a curved glass shape, the second glass piece is in a curved glass shape, the surface of the first glass piece is an upward convex curved surface, the surface of the second glass piece is an upward concave curved surface, the curvature radiuses of the surfaces of the two glass pieces to be compounded are the same, and gapless continuous contact can be achieved.
A method of compositing a first glass piece with a second glass piece comprises:
firstly, at room temperature, the first glass piece and the second glass piece are sequentially put into acetone, peroxyacetic acid solution or calcium hypochlorite solution for cleaning for 30 minutes respectively, then taken out, washed by pure water and dried. And (3) putting the cleaned first glass piece and the second glass piece into a mixed solution of sodium hypochlorite and ammonia water (the mass fractions of sodium hypochlorite, ammonia water and deionized water are 20%, 30% and 50%), treating at room temperature for 40 minutes, cleaning with pure water for 10 minutes, drying the residual solution on the surface, and activating the surface of the glass piece. The first glass piece and the second glass piece which are subjected to surface activation are contacted and heated to 250 ℃, meanwhile, the pressure of 2.0MPa is applied, the temperature and the pressure are maintained for 6 hours, and then the glass is slowly cooled, so that the glass can be partially or completely compounded together.
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is greater than 92.5%, and the obtained glass product has good optical performance and good service performance. The bonding strength was measured by the method of example 1, and the bonding strength was 130n, no change was found at the bonding position, and the glass piece was broken.
Example 7
Observing the first glass piece and the second glass piece in the glass product by naked eyesThe outer surface of the glass piece is flat and smooth without visible gaps, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, when the section is corroded in a hydrofluoric acid solution with the mass concentration of 30% for 3.5 minutes, the composite surface of the first glass piece and the second glass piece is uniformly corroded, the corrosion rate is higher than that of the first glass piece and the second glass piece, and a gap can be formed at the composite surface on the section by naked eyes.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% -93%). The first glass piece is in a curved glass shape, the second glass piece is in a curved glass shape, the surface of the first glass piece is an upward convex curved surface, the surface of the second glass piece is an upward concave curved surface, the curvature radiuses of the surfaces of the two glass pieces to be compounded are the same, and gapless continuous contact can be achieved.
A method of compositing a first glass piece with a second glass piece comprises:
firstly, organic pollution is removed from a first glass piece and a second glass piece by using an organic solvent, impurities on the surfaces of the first glass piece and the second glass piece are removed by using an alkaline cleaning agent with the pH value of 14, and the first glass piece and the second glass piece are activated by soaking in a solution with the mass fractions of 20% of sodium hypochlorite, 30% of ammonia water and 50% of deionized water at the temperature of 30 ℃ for 30 minutes.
And contacting the first glass piece and the second glass piece which are subjected to surface activation, heating to 750 ℃, simultaneously applying pressure of 0.05MPa, maintaining the temperature and the pressure for 3 hours, and slowly cooling to compound the glass partially or completely.
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is more than 91%, and the optical performance and the service performance are better. The bonding strength was measured by the method of example 1, and it was 135n, no change was found at the bonding position, and the glass piece was broken.
Example 8
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsCutting a joint position where a first glass piece and a second glass piece are connected in the glass product along the thickness direction to form a section, polishing the section, and enabling the section not to be visible with naked eyes (or composite traces) under the condition of visual observation or microscope magnification of 500 times, then contacting the section with hydrofluoric acid solution with the mass concentration of 5% for 20 minutes, corroding the contact surface of the first glass piece and the second glass piece to form a visible gap with naked eyes, wherein the width of the gap is about 20 micrometers.
The preparation method of the glass product in the embodiment comprises the following steps:
putting the cleaned first glass piece and the cleaned second glass piece (the first glass piece and the second glass piece are made of Corning GG3 glass (the visible light transmittance is 91% -93%) with the thickness of 0.7 mm) into a mixed solution with the volume ratio of ammonia water to hydrogen peroxide being (1:1), treating for 1 hour at 40 ℃, cleaning the residual solution on the surface for 10 minutes by pure water, drying, activating the surface of the glass piece, and enabling the contact angle of the activated surface of the glass piece to be not more than 5 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 550 ℃, simultaneously applying pressure of 1.0MPa, maintaining the temperature and the pressure for 3 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% for visible light (wave band 380 nm-720 nm), and the bonding strength of the glass product is tested by the method of example 1, the bonding position is unchanged, and the glass piece is broken: the bonding strength (130N) between the first glass piece or the second glass piece is not lower than the pull strength when the glass piece is pulled apart before the composite.
Example 9
The outer surfaces of the first glass piece and the second glass piece in the glass product are flat and smooth through visual observation, no visible gap exists, no obvious bubble or magic color exists at the composite position of the first glass piece and the second glass piece, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product through cutting along the thickness direction, the section is polished, no composite trace can be seen through visual observation or microscope magnification of 500 times, the composite effect is good, when the section is corroded in 10% by mass of hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, the gap can be seen through visual observation, and the gap width is 10-50 micrometers.
In this embodiment, the first glass member and the second glass member are made of corning GG3 glass (with a visible light transmittance of 91% to 93%) with a thickness of 0.7 mm.
A method of compositing a first glass piece (a sheet glass piece) and a second glass piece (a frame glass piece) comprises:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the glass pieces with pure and activated surfaces can be obtained by ultraviolet irradiation for 0.5 hour. Putting the first glass piece and the second glass piece which are subjected to surface activation into a vacuum box or a vacuum bag, and performing vacuum pumping treatment to enable the lower surface of the first glass piece to be in contact with the upper surface of the second glass piece, wherein the second glass piece can be placed on the peripheral edge of the first glass piece through a positioning method such as a positioning jig or a CCD (charge coupled device), and the like, and the second glass piece is placed on the peripheral edge of the first glass piece, wherein foreign matters or fingers cannot touch the activation surface in the placing process so as to avoid the defect of polluting the activation surface, heating to 650 ℃, applying 0.3MPa of pressure at the same time, maintaining the temperature and the pressure for 3 hours, then slowly cooling, and combining the first glass piece and the second glass piece together to obtain a glass product, wherein the structural schematic diagram is shown in FIG. 2.
In the above embodiment, the transmittance of the obtained glass product to visible light (waveband 380 nm-720 nm) is greater than 90%, and the optical performance and the service performance are better. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position is unchanged under the tensile force of 151 newtons (namely 2.1MPa), and the first glass piece and the second glass piece are broken, which shows that the two pieces of glass are compounded into a whole.
Example 10
The outer surfaces of the first glass piece and the second glass piece in the glass product are flat and smooth through visual observation, no visible gap exists, no obvious bubble or magic color exists at the composite position of the first glass piece and the second glass piece, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product through cutting along the thickness direction, the section is polished, no composite trace can be seen through visual observation or microscope magnification of 500 times, the composite effect is good, when the section is corroded in 10% by mass of hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, the gap can be seen through visual observation, and the gap width is 1-20 micrometers.
In this embodiment, the first glass member and the second glass member are made of corning GG5 glass (with a visible light transmittance of 91% to 93%) with a thickness of 1 mm.
A method of compositing a first glass piece (a sheet glass piece) and a second glass piece (a donut-shaped frame glass piece) comprising:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the glass pieces with pure and activated surfaces can be obtained by ultraviolet irradiation for 0.8 hour. And (3) contacting the first glass piece and the second glass piece with activated surfaces, heating to 700 ℃, applying 1MPa of pressure, maintaining the temperature and the pressure for 3 hours, and slowly cooling to compound the glass partially or completely to obtain the glass product, wherein the structural schematic diagram is shown in fig. 2B.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was tested according to the method of example 1 and the results were: the bonding position was unchanged under a tensile force of 156 newtons (2.16MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 11:
the outer surfaces of the first glass piece and the second glass piece in the glass product are flat and smooth and have no flesh through visual observationThe gap being visible to the eye, the first glass element and the second glass elementIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, when the section is corroded in 5 mass percent hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.1-30 micrometers.
In this embodiment, the first glass member and the second glass member are made of corning GG3 glass (with a visible light transmittance of 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece (sheet glass piece) and a second glass piece (strip glass piece) comprises:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the glass pieces with pure and activated surfaces can be obtained by ultraviolet irradiation for 0.5 hour. And (3) contacting the first glass piece and the second glass piece with activated surfaces, heating to 750 ℃, applying 2MPa of pressure, maintaining the temperature and the pressure for 4 hours, and slowly cooling to compound the glass partially or completely to obtain the glass product, wherein the structural schematic diagram is shown in figure 2C.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged under a tension of 161 n (i.e., 2.23MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 12:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe first glass piece and the second glass piece in the glass product have no obvious bubbles and fantasy colors at the composite positionAnd cutting the joint position of the parts connected along the thickness direction to form a section, polishing the section, and observing the section by visual observation or microscope magnification of 500 times without composite traces, wherein the composite effect is good, when the section is corroded in a hydrofluoric acid solution with the mass concentration of 5% for 5 minutes, the composite surface of the first glass part and the second glass part is corroded, a gap can be observed by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
The first glass piece is in a plane glass shape, the second glass piece is in a curved glass shape, and the method for compounding the first glass piece and the second glass piece comprises the following steps:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the glass pieces with pure and activated surfaces can be obtained by irradiating ultraviolet rays for 1.2 hours. The surface roughness of the glass piece surface before activation was 0.203 nm. The first glass piece and the second glass piece which are subjected to surface activation are contacted at the activated surfaces, then heated to 750 ℃, simultaneously applied with 2MPa of pressure, slowly cooled after maintaining the temperature and the pressure for 4 hours, and then the glass can be partially or completely compounded together.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged under a tension of 161 n (i.e., 2.23MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 13:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed by cutting along the thickness direction at the joint position where the first glass piece and the second glass piece are connected in the glass product, and the section is polished, visualized or displayedAnd when the section is corroded in 5% hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm. The method for compounding the first glass piece and the second glass piece comprises the following steps:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the glass pieces with pure and activated surfaces can be obtained by irradiating ultraviolet rays for 1.5 hours. The first glass piece and the second glass piece which are subjected to surface activation are contacted at the activated surfaces, then heated to 750 ℃, simultaneously applied with 2MPa of pressure, slowly cooled after maintaining the temperature and the pressure for 4 hours, and then the glass can be partially or completely compounded together.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The results of the test for the bonding strength according to the method of example 1 are: the bonding position was unchanged under a tension of 161 n (i.e., 2.23MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 14:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed by cutting along the thickness direction at the joint position where the first glass piece and the second glass piece are connected in the glass product, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, and when the section is corroded in 5 mass percent hydrofluoric acid solution for 5 minutes, the composite positions of the first glass piece and the second glass pieceThe joint is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm. The method for compounding the first glass piece and the second glass piece in gapless continuous contact comprises the following steps of:
firstly, the first glass piece and the second glass piece are cleaned by trichloroethylene for 20 minutes to clean oil stains on the surface, and then the cleaned glass is placed in a device capable of generating ozone and is irradiated by ultraviolet rays for 5 minutes. The ozone provides high-activity atomic oxygen, volatile substances are formed with free radicals generated after dirt is dissociated, active surfaces are generated, the first glass piece and the second glass piece which are subjected to surface activation are contacted at the activated surfaces, then the first glass piece and the second glass piece are heated to 750 ℃, meanwhile, 2MPa of pressure is applied, the temperature and the pressure are maintained for 4 hours, and then the glass is slowly cooled, so that the glass can be partially or completely compounded.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged under a tension of 161 n (i.e., 2.23MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 15:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished and is viewed by visual observation or microscope magnification of 500 timesWhen the section is corroded in 5% hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece and a second glass piece comprises:
firstly, cleaning a first glass piece and a second glass piece by using trichloroethylene for 20 minutes to clean surface oil stains, then placing the cleaned glass in a device capable of generating ozone, irradiating the glass for 8 minutes by using ultraviolet rays, contacting the first glass piece and the second glass piece which are subjected to surface activation at the activated surfaces, heating the glass to 750 ℃, simultaneously applying 2MPa of pressure, maintaining the temperature and the pressure for 4 hours, and then slowly cooling the glass, thus partially or completely compounding the glass.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position was unchanged under a tension of 161 n (i.e., 2.23MPa), and the first and second glass pieces broke, indicating that the two pieces of glass had fused together.
Example 16:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and magic color, a section is formed at the joint position of the first glass piece and the second glass piece in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, when the section is corroded in 5 percent hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece and a second glass piece comprises:
firstly, cleaning a first glass piece and a second glass piece by using trichloroethylene for 20 minutes to clean surface oil stains, then placing the cleaned glass in a device capable of generating ozone, irradiating the glass for 10 minutes by using ultraviolet rays, contacting the first glass piece and the second glass piece which are subjected to surface activation at the activated surfaces, heating the glass to 750 ℃, simultaneously applying 2MPa of pressure, maintaining the temperature and the pressure for 4 hours, and then slowly cooling the glass, thus partially or completely compounding the glass.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position is unchanged under the pull force of 161N, and the first glass piece and the second glass piece are broken, which shows that the two pieces of glass are fused into a whole.
Example 17:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, when the section is corroded in 5 mass percent hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece and a second glass piece comprises:
firstly, cleaning a first glass piece and a second glass piece by using trichloroethylene for 20 minutes to clean surface oil stains, then placing the cleaned glass in a device capable of generating ozone, irradiating the glass for 15 minutes by using ultraviolet rays, contacting the first glass piece and the second glass piece which are subjected to surface activation at the activated surfaces, heating the glass to 750 ℃, simultaneously applying 2MPa of pressure, maintaining the temperature and the pressure for 4 hours, and then slowly cooling the glass, thus partially or completely compounding the glass.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position is unchanged under the pull force of 161N, and the first glass piece and the second glass piece are broken, which shows that the two pieces of glass are fused into a whole.
Example 18:
observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, when the section is corroded in 5 mass percent hydrofluoric acid solution for 5 minutes, the composite surface of the first glass piece and the second glass piece is corroded, a gap can be seen by naked eyes, and the width of the gap is 0.2-2 microns.
In this embodiment, the first glass member and the second glass member are made of schottky glass (transmittance to visible light is 91% to 95%) with a thickness of 3 mm.
A method of compositing a first glass piece and a second glass piece comprises:
firstly, cleaning a first glass piece and a second glass piece by using trichloroethylene for 20 minutes to clean surface oil stains, then placing the cleaned glass in a device capable of generating ozone, irradiating the glass for 20 minutes by using ultraviolet rays, contacting the first glass piece and the second glass piece which are subjected to surface activation at the activated surfaces, heating the glass to 750 ℃, simultaneously applying 2MPa of pressure, maintaining the temperature and the pressure for 4 hours, and then slowly cooling the glass, thus partially or completely compounding the glass.
The obtained glass product has the light transmittance of more than or equal to 90 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and service performance. The bonding strength was measured according to the method of example 1, and the test results were: the bonding position is unchanged under the pull force of 161N, and the first glass piece and the second glass piece are broken, which shows that the two pieces of glass are fused into a whole.
Example 19
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd no obvious bubbles and magic color exist at the compounding position, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, no gap can be seen by naked eyes under the condition of visual observation or microscope magnification of 500 times, when the section is corroded in a hydrofluoric acid solution with the mass concentration of 40% for 2 minutes, a obvious gap can be formed at the contact surface on the section by the naked eyes, and the width of the gap is about 15 micrometers.
The preparation method of the glass product in the embodiment comprises the following steps:
cleaning the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG6 glass (the visible light transmittance is 91% -93%) with the thickness of 0.9 mm) by an erasing method or a wet method (the cleaning step is to clean the first glass piece and the second glass piece by using a mixed solution of hydrofluoric acid, sulfuric acid and a surfactant sodium dodecyl sulfate, remove oil contamination impurities and blow dry the glass pieces) and putting the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG6 glass (the visible light transmittance is 91% -93%) in a plasma cleaning machine, the excitation frequency is set to be2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2Plasma cleaning for 10 min to eliminate surface oxide and activate the surface, and contacting the activated glass surfaceThe angle is no greater than 5 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 600 ℃, simultaneously applying pressure of 0.84MPa, maintaining the temperature and the pressure for 2 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% for visible light (waveband 380 nm-720 nm), and the bonding strength of the glass product is tested by the method of example 1, the bonding position is unchanged, and the glass piece is broken: the bonding strength (140N) between the first glass piece or the second glass piece is not lower than the pull strength when the glass piece is pulled apart before the composite.
Example 20
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd no obvious bubble and magic color exist at the compounding position, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, no gap can be seen by naked eyes when the section is magnified 500 times by eyes or a microscope, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 20% for 5 minutes, a obvious gap can be formed at the contact surface on the section by the naked eyes, and the width of the gap is 20 micrometers.
The preparation method of the glass product in the embodiment comprises the following steps:
cleaning the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG3 glass (the visible light transmittance is 91% -93%) with the thickness of 0.8 mm) by an erasing method or a wet method (the cleaning step is to clean the first glass piece and the second glass piece by using a mixed solution of hydrofluoric acid, sulfuric acid and a surfactant sodium dodecyl sulfate, remove oil contamination impurities and blow dry the glass pieces) and putting the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG3 glass (the visible light transmittance is 91% -93%) into a plasma cleaning machine, the excitation frequency is set to be2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2And cleaning the surface by plasma for 10 minutes to remove oxides on the surface and activating the surface, wherein the contact angle of the surface of the glass piece after activation is not more than 5 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 450 ℃, simultaneously applying 1.0MPa of pressure, maintaining the temperature and the pressure for 3 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% for visible light (waveband 380 nm-720 nm), and the bonding strength of the glass product is tested by the method of example 1, the bonding position is unchanged, and the glass piece is broken: the bonding strength (135N) between the first glass piece or the second glass piece is not lower than the pull strength when the glass piece is pulled apart before the composite.
Example 21
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd no obvious bubbles and magic color exist at the compounding position, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, no gap can be seen by naked eyes under the condition of visual observation or microscope magnification of 500 times, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 15% for 5 minutes, a obvious gap can be formed at the contact surface on the section by the naked eyes, and the width of the gap is about 15 micrometers.
The preparation method of the glass product in the embodiment comprises the following steps:
cleaning the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG5 glass (the visible light transmittance is 91% -93%) with the thickness of 1.0 mm) by an erasing method or a wet method (the cleaning step is to clean the first glass piece and the second glass piece by using a mixed solution of hydrofluoric acid, sulfuric acid and surfactant sodium dodecyl sulfate, remove oil contamination impurities and blow dry the glass pieces), putting the first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2And cleaning the surface by plasma for 10 minutes to remove oxides on the surface and activating the surface, wherein the contact angle of the surface of the glass piece after activation is not more than 5 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 250 ℃, simultaneously applying 2.0MPa of pressure, maintaining the temperature and the pressure for 3 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% for visible light (waveband 380 nm-720 nm), and the bonding strength of the glass product is tested by the method of example 1, the bonding position is unchanged, and the glass piece is broken: the bonding strength (130N) between the first glass piece or the second glass piece is not lower than the pull strength when the glass piece is pulled apart before the composite.
Example 22
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd no obvious bubbles and magic color exist at the compounding position, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, no gap can be seen by naked eyes under the condition of visual observation or microscope magnification of 500 times, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 30% for 3.5 minutes, a obvious gap can be formed at the contact surface on the section by naked eyes, and the width of the gap is about 20 micrometers.
The preparation method of the glass product in the embodiment comprises the following steps:
cleaning the first glass piece and the second glass piece (the first glass piece and the second glass piece are made of corning GG5 glass (the visible light transmittance is 91% -93%) with the thickness of 1.2 mm) by an erasing method or a wet method (the cleaning step is to clean the first glass piece and the second glass piece by using a mixed solution of hydrofluoric acid, sulfuric acid and surfactant sodium dodecyl sulfate, remove oil contamination impurities and blow dry the glass pieces), putting the first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2And cleaning the surface by plasma for 10 minutes to remove oxides on the surface and activating the surface, wherein the contact angle of the surface of the glass piece after activation is not more than 5 degrees.
And laminating the first glass piece and the second glass piece which are subjected to surface activation, heating to 750 ℃, simultaneously applying pressure of 0.05MPa, maintaining the temperature and the pressure for 3 hours, and slowly cooling to partially or completely compound the glass together.
The obtained glass product has a light transmittance of more than 91% for visible light (waveband 380 nm-720 nm), and the bonding strength of the glass product is tested by the method of example 1, the bonding position is unchanged, and the glass piece is broken: the bonding strength (135N) between the first glass piece or the second glass piece is not lower than the pull strength when the glass piece is pulled apart before the composite.
Example 23
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd the composite position has no obvious bubbles and magic colors, a section is formed at the joint position of the first glass piece and the second glass piece in a cutting mode along the thickness direction, the section is polished, and no composite trace or gap can be seen visually or under the condition of microscope magnification of 500 times, so that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 30% for 3 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2And (3) cleaning the surface for 10 minutes by using plasma, removing organic matters on the surface and activating the surface.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 129 newtons (namely 1.8MPa), the bonding position is unchanged, and the glass piece is broken.
Example 24
Observing the first glass piece and the second glass piece in the glass product by naked eyesThe outer surface of the glass piece is flat and smooth without visible gaps, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 20% for 4 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and utilizing N2/H2The plasma cleaning is carried out for 10 minutes to remove the oxide on the surface and carry out surface activation.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 131N (namely 1.82MPa), the bonding position is unchanged, and the glass piece is broken.
Example 25
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd the composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which indicates that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 15% for 7 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except thatIn the following steps: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 5 min to remove organic matter on the surface, and reusing N2/H2The plasma cleaning was carried out for 5 minutes to remove the oxide on the surface and to activate the surface.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 145 newtons (namely 2.0MPa), the bonding position is unchanged, and the glass piece is broken.
Example 26
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd the composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which indicates that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 25% for 8 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2The plasma cleaning was carried out for 5 minutes to remove the oxide on the surface and to activate the surface.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass piece is tested, and the result shows that the bonding strength is 148 newtons (namely 2.05MPa), the bonding position is unchanged, and the glass piece is broken.
Example 27
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsAnd the composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which indicates that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 35% for 5 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 5 min to remove organic matter on the surface, and reusing N2/H2The plasma cleaning is carried out for 10 minutes to remove the oxide on the surface and carry out surface activation.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 149 newtons (namely 2.06MPa), the bonding position is unchanged, and the glass piece is broken.
Example 28
Observing the first and second glass pieces in the glass product by naked eyes that the outer surfaces are flat and smooth without visible gaps by naked eyesA glass member and a second glass memberIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, and when the section is corroded in 10 percent hydrofluoric acid solution for 10 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The glass article was prepared in the same manner as in example 19 except that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Plasma cleaning for 10 min to eliminate organic matter from the surface and reuse N2/H2The plasma cleaning was carried out for 15 minutes to remove the oxide on the surface and to activate the surface.
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. And the bonding strength is tested, and the result shows that the bonding strength is 150 newtons (namely 2.08MPa), the bonding position is unchanged, and the glass piece is broken.
Example 29
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, and when the section is corroded in a hydrofluoric acid solution with the mass concentration of 5% for 10 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
Preparation of glass articles19, the difference is that: the cleaning treatment and the activation treatment steps are as follows: and at room temperature, sequentially putting the first glass piece and the second glass piece into acetone, peroxyacetic acid solution or calcium hypochlorite solution, respectively cleaning for 30 minutes, taking out, washing with pure water, and drying. Then putting the cleaned first glass piece and the second glass piece into a plasma cleaning machine, setting the excitation frequency to be 13.56MHz, and using O2Cleaning with plasma for 15 min to remove organic substances on the surface, and recycling N2/H2The plasma cleaning was carried out for 15 minutes to remove the oxide on the surface and to activate the surface. .
In the embodiment, the light transmittance of the obtained glass product to visible light (the wave band is 380 nm-720 nm) is more than 91%, and the obtained glass product has better optical performance and better service performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 151 newtons (namely 2.10MPa), the bonding position is unchanged, and the glass piece is broken.
Example 30
Observing the first glass piece and the second glass piece in the glass product by naked eyes, wherein the outer surfaces of the first glass piece and the second glass piece are flat and smooth and have no visible gaps with naked eyes, and the first glass piece and the second glass pieceIs/are as followsThe composite position has no obvious bubbles and fantasy colors, a section is formed at the joint position where the first glass piece and the second glass piece are connected in the glass product by cutting along the thickness direction, the section is polished, and no composite trace or gap can be seen by visual observation or microscope magnification of 500 times, which shows that the composite effect is good, and when the section is corroded in 5% by mass of hydrofluoric acid solution for 10 minutes, an obvious gap can be formed at the composite surface on the section by naked eyes.
The preparation method of the glass product is the same as that in example 19, except that the first glass piece is in the shape of curved glass, the second glass piece is in the shape of curved glass, the surface of the first glass piece is an upward convex curved surface, the surface of the second glass piece is an upward concave curved surface, and the curvature radii of the surfaces of the two glass pieces to be compounded are the same, so that gapless continuous contact can be achieved.
The obtained glass product has the light transmittance of more than 91 percent to visible light (the wave band is 380 nm-720 nm), and has better optical performance and use performance. The bonding strength of the glass is tested, and the result shows that the bonding strength is 140 newtons (namely 1.94MPa), the bonding position is unchanged, and the glass piece is broken.
Comparative example 1
A glass article was prepared according to the method of example 1, except that the first glass piece and the second glass piece were not subjected to an activation treatment. The obtained glass product was observed to have a remarkable glittering color and large bubbles (see fig. 20), and the bonding strength was measured by the method of example 1, the bonding strength was 10 n, the glass product was cut in the vertical direction of the composite plane, the composite plane had a composite gap at the position where the glittering color of bubbles was present (see fig. 21), and the glass product was broken by dropping a steel ball of 32 g from a height of 1m, and the glass partially cracked at the position of the composite plane, indicating that the composite effect was not good. The bonding strength of the bubbles and the multicolor part is poor, and the bubbles and the multicolor part are easy to break. The bonding strength of the bubbles and the colorful parts is poor, the bubbles and the colorful parts are easy to break, and the use requirement of the shell of the electronic equipment can not be met.
Comparative example 2
A glass article was prepared according to the method of example 1, except that no activation treatment was performed, and the first glass piece and the second glass piece were laminated and heated to a temperature above the softening point of the first glass piece and the second glass piece. Obvious indentation and die marks can be seen on the obtained glass product composite surface through observation, the deformation is serious, the light transmittance of visible light (the wave band is 380 nm-720 nm) is only about 85%, the local transmittance is less than or equal to 75%, the optical performance is seriously influenced, and the bonding strength is tested by the testing method of the embodiment 1 and is basically consistent with that of the embodiment 1. When the glass product is cut along the vertical direction of the composite plane and corroded in a hydrofluoric acid solution with the mass concentration of 40% for 2 minutes, no gap is visible to naked eyes at the composite plane, and the method can obtain the same composite effect but cannot meet the appearance requirement.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (11)

1. A method of inspecting a glass article, comprising:
(1) carrying out surface detection on a sample to be detected, and selecting the sample to be detected with no visible gap on the surface to enter the step (2);
(2) contacting the surface of the sample to be tested with an acidic reagent, and after the contacting, performing secondary surface detection on the sample to be tested, wherein the occurrence of a gap on the surface of the sample to be tested after the contacting is an indication that the sample to be tested is prepared by a low-temperature fusion process and the sample to be tested has a predetermined binding strength.
2. The method of claim 1, wherein the surface is detected as a visual observation or an observation with a magnifying glass or microscope.
3. The method of claim 2, wherein the surface is detected as viewed with a magnifying glass or microscope at least 100 times magnification.
4. The method of claim 1, wherein the surface is detected as viewed with a magnifying glass or microscope at a magnification of at least 300.
5. The method of claim 1, wherein the surface is detected as viewed with a magnifying glass or microscope at a magnification of at least 500.
6. The method of claim 1, wherein the acidic solution is a hydrofluoric acid solution.
7. The method according to claim 6, wherein the acidic solution is a hydrofluoric acid solution having a mass concentration of 5% to 40%.
8. The method according to claim 7, wherein the sample to be tested is contacted with hydrofluoric acid solution with mass concentration of 5% -40% for 30 seconds to 20 minutes, and the appearance of the gap with width of 0.1-300 μm on the surface of the sample to be tested is an indication that the sample to be tested is prepared by low temperature fusion process and the sample to be tested has predetermined binding strength.
9. The method of claim 8, wherein any one of the following (a) to (h) is indicative that the sample to be tested is prepared for a low temperature fusion process and the sample to be tested has a predetermined binding strength:
(a) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 5% for 300 seconds, wherein the width of the gap is 0.1-30 microns;
(b) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 10% for 300 seconds, wherein a gap with the width of 0.5-50 microns is formed on the surface of the sample to be detected;
(c) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 20% for 300 seconds, wherein a gap with the width of 0.5-100 micrometers appears on the surface of the sample to be detected;
(d) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 40% for 300 seconds, wherein the gap with the width of 2-100 micrometers appears on the surface of the sample to be detected;
(e) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 5% for 600 seconds, wherein a gap with the width of 1-50 microns is formed on the surface of the sample to be detected;
(f) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 10% for 600 seconds, wherein a gap with the width of 1-80 microns is formed on the surface of the sample to be detected;
(g) contacting the sample to be detected with hydrofluoric acid with the mass concentration of 20% for 600 seconds, wherein a gap with the width of 3-120 microns is formed on the surface of the sample to be detected;
(h) and contacting the sample to be detected with hydrofluoric acid with the mass concentration of 40% for 600 seconds, wherein the gap with the width of 5-120 microns is formed on the surface of the sample to be detected.
10. The method according to any one of claims 1-9, wherein the sample to be tested comprises a first glass piece and a second glass piece connected at least partially on their surfaces, the contact position of the first glass piece and the second glass piece defining a contact surface, and wherein after the contact, the presence of a gap in the surface of the sample to be tested and the gap extending along the contact surface is indicative of the sample to be tested being prepared for a low temperature fusion process and the sample to be tested having a predetermined bond strength.
11. The method of claim 10, wherein the method comprises:
(1-1) cutting the sample to be detected in a direction forming a preset angle with the contact surface to obtain a cut surface;
(1-2) carrying out surface detection on the cut surface, and selecting the sample to be detected with no visible gap on the surface to enter the step (1-3);
(1-3) contacting the cut surface with an acidic reagent and performing the secondary surface inspection on the cut surface after the contacting, wherein after the contacting, the appearance of a gap in the surface of the cut surface and the extension of the gap along the contact surface are indicative that the sample to be tested is prepared for a low temperature fusion process and the sample to be tested has a predetermined bond strength.
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