Glass photoresist removing liquid as well as preparation method and application thereof

Abstract

The invention provides a glass photoresist removing solution as well as a preparation method and application thereof. The glass photoresist removing solution is prepared from the following components in parts by weight: 10 to 20 parts of a flexible glue solvent, 5 to 10 parts of a penetrant, 6 to 12 parts of a solubilizer, 1 to 3 parts of a protective agent and 60 to 80 parts of water. The glass degumming liquid provided by the invention is mild in use condition and good in degumming effect, and glass after degumming is high in cleanliness, low in scratch rate and high in visible light transmittance.

Description

Technical Field

[0001] The invention belongs to the technical field of glass processing, and specifically relates to a glass degumming liquid and a preparation method and application thereof, and in particular to a glass degumming liquid with high cleanliness and a preparation method and application thereof. Background Art

[0002] The development of communication technology has brought about the continuous iteration of the ICT ecosystem. As a user-side carrier, mobile terminals continue to upgrade in the 5G era. The market demand for foldable devices, mobile phones, bracelets, TVs, smart screens, AR / VR, etc. has grown dramatically. In order to fully realize flexible display, the display cover part should have the characteristics of being repeatedly bendable, transparent, ultra-thin, and sufficiently hard. Ultra-thin flexible glass UTG has become the mainstream choice for display cover materials due to its own material flexibility, high strength and durability, good touch, excellent impact resistance, and high light transmittance. In the edge processing process of ultra-thin flexible glass UTG, whether it is stacked or single-piece processing, it is necessary to coat UV protective glue, and then go through CNC trimming, SPM polishing, pickling and chamfering, hydrolysis of UV protective glue, chemical strengthening and other process flows. At present, the process has the problem of incomplete removal of UV protective glue residue after hydrolysis, resulting in in-plane etching pits after chemical strengthening, resulting in low processing yield.

[0003] CN113306270B discloses an ultra-thin glass thinning and debonding separation device, which includes a tank body and a blue tool mechanism; the tank body is provided with a heating element, and the heating element is used to heat the liquid contained in the tank body; the blue tool mechanism is detachably arranged on the tank body, and the blue tool mechanism is used to clamp the glass to be separated. When the glass to be separated is subjected to UV glue separation, the UV glue can be separated by immersing the glass to be separated into the tank body through the blue tool mechanism. When the device is used for UV glue separation, the fragmentation rate is greatly reduced, the debonding rate is high, the use time is short, and no odor is generated. However, this method requires the use of special equipment, and it uses water as the debonding liquid, which is prone to residue.

[0004] CN105149309A discloses a degumming process for optical glass glued lenses, which is as follows: 1. After the lens is aligned with the optical axis, it is fixed with UV light. The glue undergoes a chemical reaction and solidifies after being exposed to ultraviolet light, and the cured glue will remain around the lens; 2. The glued lenses are directly placed on the cleaning bar; 3. The lenses on the cleaning bar are directly placed in the BOLI-3 cleaning solution and soaked for about 15 minutes; 4. After soaking in BOLI-3, the lenses can be washed in an ultrapure water system for 3 minutes; the invention has a short degumming time and a significant effect. It is non-destructive to the glue gap and does not harm the lens. However, it does not involve the residual problem of degumming, nor does it provide relevant solutions.

[0005] Since the existing process has problems such as incomplete removal and damage to the glass surface, how to provide a degumming method with high processing yield, small residue and no scratches on the glass has become an urgent problem to be solved. Summary of the invention

[0006] In view of the shortcomings of the prior art, the object of the present invention is to provide a glass degumming liquid and a preparation method and application thereof, in particular to provide a glass degumming liquid with high cleanliness and a preparation method and application thereof. The glass degumming liquid provided by the present invention has mild use conditions and good degumming effect. After degumming, the glass has high cleanliness, low scratch rate and high visible light transmittance.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a glass degumming liquid, which comprises, by weight, 10-20 parts of a soft glue solvent, 5-10 parts of a penetrant, 6-12 parts of a solubilizer, 1-3 parts of a protective agent, and 60-80 parts of water.

[0009] Among them, the number of parts of the soft glue solvent can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts or 20 parts, etc., the number of parts of the penetrant can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts, etc., the number of parts of the solubilizer can be 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts or 12 parts, etc., the number of parts of the protective agent can be 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts, etc., the number of parts of water can be 60 parts, 65 parts, 70 parts, 75 parts or 80 parts, etc., but are not limited to the values ​​listed above, and other values ​​not listed within the above numerical range are equally applicable.

[0010] The above-mentioned glass degumming liquid adopts a compound of soft glue solvent, penetrant and solubilizer, which work synergistically and can effectively enhance the degumming effect, improve the cleanliness of the glass after degumming, reduce the scratch rate, and increase the visible light transmittance. The product has mild use conditions (when used to remove ultra-thin flexible glass UV protective glue, the use temperature is 40-60°C and the time is 10-20min), saving process time and energy consumption.

[0011] Preferably, the soft gel solvent includes any one of limonene, phellandrene or pinene, or a combination of at least two of them.

[0012] Preferably, the soft gel solvent is a combination of limonene and pinene.

[0013] The above-mentioned specific soft glue solvent combination can further improve the effect of the product compared with other options; at the same time, compared with ingredients such as sodium hydroxide in the prior art, the above-mentioned specific soft glue solvent can make the product neutral, more environmentally friendly and safe, and can effectively reduce the micro-scratch rate of ultra-thin flexible glass after processing.

[0014] Preferably, the penetrant includes any one of diethylene glycol monobutyl ether, ethylene glycol monobutyl ether, propylene glycol monobutyl ether or dipropylene glycol butyl ether, or a combination of at least two thereof.

[0015] Preferably, the penetrant is a combination of ethylene glycol monobutyl ether and propylene glycol monobutyl ether.

[0016] The above-mentioned specific penetrant combination can form a directional arrangement on the surface of the solution, significantly reducing the surface tension of the glass, and has a strong penetrating effect, which can further improve the effect of the product compared with other options.

[0017] Preferably, the solubilizer includes any one of ethylene glycol, propylene glycol, glycerol or diethylene glycol, or a combination of at least two thereof.

[0018] Preferably, the solubilizer is a combination of propylene glycol and glycerol.

[0019] The above-mentioned specific solubilizer combination can form micelles in the solution, increase the solubility of the poorly soluble components in the solution, and form a uniform solution, which can further improve the effect of the product compared with other options.

[0020] Preferably, the protective agent includes any one of sodium lignin sulfonate, sodium alginate or xanthan gum, or a combination of at least two thereof, preferably sodium lignin sulfonate.

[0021] Compared with existing inorganic salt reagents, the above-mentioned specific protective agent can effectively protect the glass surface and reduce the micro-scratch rate of ultra-thin flexible glass after processing.

[0022] In a second aspect, the present invention provides a method for preparing the glass degumming solution as described above, the preparation method comprising the following steps:

[0023] The glass degumming liquid is obtained by mixing water with a soft glue solvent and a penetrant, and then mixing with a solubilizer and a protective agent.

[0024] In a third aspect, the present invention provides application of the glass degumming liquid as described above in processing ultra-thin flexible glass.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The present invention provides a glass degumming liquid, which can effectively enhance the degumming effect, improve the cleanliness of the glass after degumming, reduce the scratch rate, and improve the visible light transmittance by compounding a soft glue solvent, a penetrant, and a solubilizer. The product has mild use conditions and saves process time and energy consumption. DETAILED DESCRIPTION

[0027] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0028] Example 1

[0029] This embodiment provides a glass degumming solution, the specific components of which are as follows (in mass percentage):

[0030] Limonene 10%, pinene 5%, ethylene glycol monobutyl ether 5%, propylene glycol monobutyl ether 3%, propylene glycol 4%, glycerol 4%, sodium lignin sulfonate 1.5%, and deionized water as the balance.

[0031] The preparation method is as follows:

[0032] Deionized water is added to a disperser, and limonene, pinene, ethylene glycol monobutyl ether, and propylene glycol monobutyl ether are accurately weighed, and a first stirring is performed until they are completely dispersed, with a rotation speed of 800 r / min and a time of 15 min; then propylene glycol, glycerol, and sodium lignin sulfonate are added, and a second stirring is performed, with a rotation speed of 1200 r / min and a time of 40 min, to obtain the glass degumming liquid.

[0033] Example 2

[0034] This embodiment provides a glass degumming solution, the specific components of which are as follows (in mass percentage):

[0035] Limonene 5%, pinene 5%, ethylene glycol monobutyl ether 5%, propylene glycol monobutyl ether 5%, propylene glycol 4%, glycerol 2%, sodium alginate 3%, and deionized water as the balance.

[0036] The preparation method is similar to that of Example 1.

[0037] Example 3

[0038] This embodiment provides a glass degumming solution, the specific components of which are as follows (in mass percentage):

[0039] Limonene 10%, pinene 10%, ethylene glycol monobutyl ether 3%, propylene glycol monobutyl ether 2%, propylene glycol 6%, glycerol 6%, xanthan gum 1%, and the balance deionized water.

[0040] The preparation method is similar to that of Example 1.

[0041] Example 4

[0042] This embodiment provides a glass degumming solution, and the specific ingredients are the same as those of Embodiment 1 except that limonene is replaced by an equal amount of pinene.

[0043] The preparation method is similar to that of Example 1.

[0044] Example 5

[0045] This embodiment provides a glass degumming solution, and the specific ingredients are the same as those of Embodiment 1 except that pinene is replaced with an equal amount of limonene.

[0046] The preparation method is similar to that of Example 1.

[0047] Example 6

[0048] This embodiment provides a glass degumming liquid, and the specific components are the same as those of Embodiment 1 except that ethylene glycol monobutyl ether is replaced by an equal amount of propylene glycol monobutyl ether.

[0049] The preparation method is similar to that of Example 1.

[0050] Example 7

[0051] This embodiment provides a glass debonding solution, and the specific components are the same as those of Embodiment 1 except that propylene glycol monobutyl ether is replaced by an equal amount of ethylene glycol monobutyl ether.

[0052] The preparation method is similar to that of Example 1.

[0053] Example 8

[0054] This embodiment provides a glass degumming liquid, and the specific components are the same as those of Embodiment 1 except that propylene glycol is replaced by an equal amount of propylene glycol.

[0055] The preparation method is similar to that of Example 1.

[0056] Example 9

[0057] This embodiment provides a glass degumming liquid, and the specific components are the same as those of Embodiment 1 except that propylene glycol is replaced with propylene glycol in an equal amount.

[0058] The preparation method is similar to that of Example 1.

[0059] Comparative Example 1

[0060] This comparative example provides a glass degumming liquid, which is consistent with Example 1 except that limonene and pinene are not included and the reduced portion is distributed proportionally to ethylene glycol monobutyl ether, propylene glycol monobutyl ether, propylene glycol and glycerol.

[0061] The preparation method is similar to that of Example 1.

[0062] Comparative Example 2

[0063] This comparative example provides a glass degumming liquid, which is consistent with Example 1 except that ethylene glycol monobutyl ether and propylene glycol monobutyl ether are not included and the reduced portion is proportionally distributed to limonene, pinene, propylene glycol and glycerol.

[0064] The preparation method is similar to that of Example 1.

[0065] Comparative Example 3

[0066] This comparative example provides a glass degumming liquid, and the specific components thereof are consistent with those of Example 1 except that propylene glycol and glycerol are not included and the reduced portions are distributed proportionally to ethylene glycol monobutyl ether, propylene glycol monobutyl ether, limonene and pinene.

[0067] The preparation method is similar to that of Example 1.

[0068] Comparative Example 4

[0069] This comparative example provides a glass degumming solution, and the specific ingredients are the same as those in Example 1 except that limonene and pinene are replaced by an equal amount of sodium hydroxide.

[0070] The preparation method is similar to that of Example 1.

[0071] Effect test:

[0072] The glass degumming solutions provided in Examples 1-9 and Comparative Examples 1-4 were tested respectively, and the testing methods were as follows:

[0073] Add glass degumming liquid into the degumming immersion tank equipment; use the degumming liquid to remove the UV protective glue of the ultra-thin flexible glass, the degumming liquid is used at a temperature of 50°C and the time is 20 minutes, and the ultra-thin flexible glass after degumming is cleaned and dried.

[0074] 5000 pieces of glue were removed from each embodiment and comparative example respectively. After the degumming was completed, the surface cleanliness of the ultra-thin flexible glass was detected using a German SITA surface cleanliness meter (10 points were taken, the diameter of each point was 1mm, and the average value of the 10 points was tested). The average value of RFU (related fluorescence unit) obtained by the test was ≤50RFU, which was judged to be qualified in cleanliness, otherwise it was unqualified, and the yield rate = (the number of glasses with an average value of RFU ≤50 / the total number of glasses invested) × 100%; the scratch detection method was visual inspection, and any point-shaped or stripe-shaped scratches on the glass were defined as defective, and the micro-scratch rate = (the number of defective glasses / the total number of glasses invested) × 100%; the transmittance measuring instrument LS108A of Shenzhen Linshang Technology was used to measure the transmittance of the ultra-thin flexible glass at a visible light peak wavelength of 550nm (3 points were taken, and the average value of the 3 points was tested), and the total average value was calculated.

[0075] The results are as follows:

[0076] Group Cleanliness yield Micro scratch rate Visible light transmittance Example 1 99.5％ 0.1％ 91.8％ Example 2 99％ 0.15％ 91.5％ Example 3 99％ 0.1％ 91.5％ Example 4 98.8％ 0.2％ 91.2％ Example 5 98.6％ 0.22％ 91.0％ Example 6 98.5％ 0.25％ 90.8％ Example 7 98.2％ 0.27％ 90.5％ Example 8 98.6％ 0.22％ 91.0％ Example 9 98.5％ 0.25％ 90.8％ Comparative Example 1 78％ 0.15％ 85.0％ Comparative Example 2 76％ 0.22％ 84.2％ Comparative Example 3 80％ 0.20％ 87.5％ Comparative Example 4 98.5％ 8％ 76.0％

[0077] From the above results, it can be found that the glass degumming liquid provided by the present invention can effectively remove the ultra-thin flexible glass UV protective glue, and has the characteristics of good degumming effect, low residue, low micro-scratch rate and high visible light transmittance; By comparing Examples 1-9, it can be found that the present invention can further improve the effect of the product by selecting specific soft glue solvents, penetrants and solubilizers; By comparing Example 1 and Comparative Examples 1-3, it can be found that the present invention adopts a compound of soft glue solvents, penetrants and solubilizers, and the synergistic effect can effectively enhance the degumming effect, improve the cleanliness of the glass after degumming, reduce the scratch rate, and improve the visible light transmittance; By comparing Example 1 and Comparative Example 4, it can be found that compared with the existing degumming agent components, the present invention has less scratches on the glass surface and higher visible light transmittance.

[0078] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the glass degumming liquid and its preparation method and application, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0079] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0080] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A glass degumming liquid, characterized in that: The glass debonding solution comprises, by weight, 10-20 parts of a soft glue solvent, 5-10 parts of a penetrant, 6-12 parts of a solubilizer, 1-3 parts of a protective agent and 60-80 parts of water.

2. The glass degumming liquid according to claim 1, characterized in that: The soft gel solvent includes any one of limonene, phellandrene or pinene, or a combination of at least two of them.

3. The glass degumming liquid according to claim 2, characterized in that: The soft gel solvent is a combination of limonene and pinene.

4. The glass degumming solution according to any one of claims 1 to 3, characterized in that: The penetrant includes any one of diethylene glycol monobutyl ether, ethylene glycol monobutyl ether, propylene glycol monobutyl ether or dipropylene glycol butyl ether, or a combination of at least two of them.

5. The glass degumming liquid according to claim 4, characterized in that: The penetrant is a combination of ethylene glycol monobutyl ether and propylene glycol monobutyl ether.

6. The glass degumming solution according to any one of claims 1 to 5, characterized in that: The solubilizer includes any one of ethylene glycol, propylene glycol, glycerol or diethylene glycol, or a combination of at least two of them.

7. The glass degumming liquid according to claim 6, characterized in that: The solubilizer is a combination of propylene glycol and glycerol.

8. The glass degumming solution according to any one of claims 1 to 7, characterized in that: The protective agent includes any one of sodium lignin sulfonate, sodium alginate or xanthan gum or a combination of at least two thereof, preferably sodium lignin sulfonate.

9. A method for preparing a glass degumming solution according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: The glass degumming liquid is obtained by mixing water with a soft glue solvent and a penetrant, and then mixing with a solubilizer and a protective agent.

10. Use of the glass degumming liquid according to any one of claims 1 to 8 in processing ultra-thin flexible glass.