CN105645785A - Method for reinforcing high-strength protective glass - Google Patents

Abstract

The invention discloses a method for reinforcing high-strength protective glass. The method includes steps of carrying out edge polishing, chamfering and punching treatment on the glass by the aid of an engraving machine; ultrasonically cleaning the glass and carrying out micro-etching treatment and chemical reinforcing treatment on the glass. The method further includes a step of carrying out chemical reinforcing pretreatment on the glass. The chemical reinforcing pretreatment can be carried out on the glass after the punching treatment and before the glass is ultrasonically cleaned or between the micro-etching treatment and the chemical reinforcing treatment. The method has the advantages that tin-doped layers and micro-crack on glass surface layers can be removed, double chemical reinforcing processes and a micro-etching process are combined with one another, and accordingly the glass can be greatly enhanced.

Description

The enhancement method of a kind of high strength protective glass

Technical field

The present invention relates to glass reinforced field, say the enhancement method relating to a kind of high strength protective glass more specifically.

Background technology

Along with the high speed development of intelligent touch industry, there are two big technical tasks towards display device protection glass substrate at present. One be the thickness of glass to thinning transition, existing 0.70��0.40mm glass is the main product of cover plate protective glass, wherein again taking the ultra-thin glass of 0.40mm as leading technology. Another is then the surface strength performance of glass, and its intensity of glass of more thinning can reduce than heavy sheet glass in chemical enhanced rear intensity usually, also just means that the mobile phone with its assembling is more easy and is broken into pieces.

At present have to pass through the edging of essence carving machine, chamfering, punching process as display device protection glass. What carve that machine adopts due to essence is that glass is processed by the main shaft of high speed rotating, needing to be fixed by glass, what fixing method adopted is vacuum suck, draws wound to prevent simultaneously, adsorption plane is carried out aluminum coated steel, and this just causes glass surface and easily leaves sucker trace and film vestige. Naked eyes are almost invisible in normal circumstances for these traces, but visible under the high light of darkroom.

The factor affecting strength of glass is mainly: glass surface tiny crack and glass surface ooze tin. Adopt etching method can remove these two kinds of factors to the impact of strength of glass. The general one side etched thickness of traditional method is 80��150 ��m, removes while oozing tin layers and crizzle, also reduces the thickness of glass. Along with the increase of etched thickness, the homogeneity of glass surface can not ensure, also to be carried out polished finish after causing etching, and cost increases greatly. The operations such as the glass after simultaneously having etched also to cut through cutting machine, essence carving machine grinding, cause the appearance again of glass surface tiny crack, finally cause chemical enhanced after strength of glass reduce.

Based on above-mentioned background, it is desirable to while removing glass surface trace, reduce the etched thickness of glass, increase substantially the surface strength of chemical enhanced rear glass.

Summary of the invention

The present invention provides a kind of while removing glass surface trace, reduces the etched thickness of glass, increases substantially the enhancement method of the surface strength of chemical enhanced rear glass.

For solving above-mentioned technical problem, the present invention by the following technical solutions:

The enhancement method of a kind of high strength protective glass; glass is carried out after edging, chamfering, punching process through essence carving machine; carry out ultrasonic cleaning, microetch process, chemical intensification treatment again; also comprise chemical enhanced pre-treatment step, chemical enhanced pre-treatment can essence carve machine carry out edging, chamfering, punching process after, before ultrasonic cleaning or between microetch process and chemical intensification treatment.

Aforesaid method, the performance of the chilled glass that the processing method of employing prior art obtains just has lifting to a certain degree. Glass reinforced field is a positive factor by this.

Prior art be all follow the prescribed order glass is carried out edging, chamfer machining after, carry out chemical intensification treatment again, this kind of method also can obtain chilled glass, but the degree of depth that the chilled glass that this kind of method obtains etches relatively big (general one side can reach 80��150 ��m), the intensity that can bear is not high, the homogeneity of glass surface is not good, also to be carried out polished finish, too increase cost after causing etching. in glass reinforced field, owing to glass reinforced method is physics and chemistry method two class, physical method mainly adopts mechanical means, chemical process then adopts the method such as ion-exchange or acidifying, according to general thinking, glass reinforced influence factor is main relevant with chemical enhanced technique, and general employing reinforcing process adds that other such as clean additional step. therefore, the technique of other additional step such as reinforcing process and cleaning is substantially set. having very big difference with prior art, the present invention adopts chemical enhanced pre-treatment, microetch process, chemical intensification treatment and other supplementary meanss to combine, it is possible to obtain the glass that intensity is higher, and contriver accidentally finds in experimentation, chemical enhanced pretreated technique position difference and whole process sequence are different, the glass properties obtained after glass reinforced also can be different, and chemical enhanced pre-treatment is placed on essence carving machine and carries out edging, chamfering, after punching processes, effect before ultrasonic cleaning or between microetch process and chemical intensification treatment is consistent, the characteristic of the chilled glass obtained all is greatly improved, namely strengthening the chilled glass bearing stress obtained is 820��880Mpa, the compressive stress layer degree of depth is 30��50 ��m, relative to prior art, the technique of the present invention and the chilled glass obtained have outstanding substantive distinguishing features and significant progress.

The microetch medium that microetch process uses comprises following component, represents with mass percent, HF:1%��5%, H₂SO₄: 1%��8%, HNO₃: 0%��5%, HF+H simultaneously₂SO₄+HNO₃+ HCL total amount 7%��12%, all the other are pure water.

In the present invention, HF is in microetch process, the SiO mainly and in glass₂��MgO��Na₂O etc. react, and play and peel off the effect that glass oozes tin layers and crizzle; H₂SO₄In polishing process, the insoluble silicofluoride formed when HF degrades glass surface is dissolved in main effect, avoids its residue to adhere to glass surface, makes the glass surface after process smooth, therefore HF+H₂SO₄+HNO₃+ HCL total amount represents with mass percent and should control 7%��12%.

Microetch process is specially: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media.

The microetch treatment time is 2��15min. Microetch technique can control the etch depth of glass, the strengthening performance of glass is influential, it is intended to control the etch depth of different glass, need to adjust group part of microetch medium and rationally arrange the microetch treatment time.

Ultrasonic cleaning is specially and washes at the beginning of the alkali lye with 8-10wt%, and scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again. Alkali lye can be the common alkali lye such as sodium hydroxide, sodium carbonate.

Owing to glass is carved in machining process in essence, the dual reason of vacuum suck and overlay film, causes glass surface naked eyes invisible darkroom high light visible trace occur.

The present invention adopts the method for Chemical Pretreatment can remove the above trace, is positioned over by glass in saltpetre fused salt and carries out high temperature pre-treatment, and pretreatment temperature is 380 DEG C��400 DEG C, and the chemical enhanced time is 2��30min. Wherein, pretreatment temperature is preferably 390 DEG C��400 DEG C, and the chemical enhanced time is preferably 2��10min.

Chemical intensification treatment is specially to be put into glass tempering liquid and carries out chemical enhanced, and chemical enhanced temperature is 380 DEG C��430 DEG C, and the chemical enhanced time is 4��8 hours. There is mutual exchange in the alkalimetal ion in glass and the alkalimetal ion in fused salt, produce " jammed " phenomenon because of diffusion, makes glass surface produce stress under compression, thus improves the intensity of glass.

The chilled glass that foregoing enhancement method is obtained, double-sided glass microetch thickness is 18��25 ��m, and chemically reinforced glass bearing stress is 820��880Mpa, and the compressive stress layer degree of depth is 35��50 ��m.

Research finds: when the tin amount of oozing of glass surface reaches to a certain degree, the tin infiltrating glass surface can change the chemistry composition of surface layer of glass, also can as network modification ion, change the network structure of glass surface, also it is exactly the physical and chemical performance changing glass surface, thus the performances such as the mechanics of glass, optics are caused impact. Therefore, ooze tin layers and the existence of glass surface tiny crack, cause chemical enhanced after actual glass intensity reduce significantly.

Enhancement method set forth in the present invention makes the thickness of etching glass remain on two-sided 18��25 ��m, what eliminate surface layer of glass oozes tin layers and tiny crack, the chemical enhanced pretreated glass of employing can be removed the compressive stress layer degree of depth (5��10 ��m) and glass surface stress simultaneously. By the glass of chemical enhanced pre-treatment, microetch process, chemical intensification treatment, after chemical enhanced, intensity is greatly improved.

Representing with mass percent, chilled glass comprises following component: SiO₂: 60��65%, Al₂O₃: 11��17%, K₂O:0.2%��6.8%, ZrO₂: 0%��1.8%, SiO simultaneously₂+Al₂O₃+Na₂O+K₂O+MgO+ZrO₂The total amount of+CaO represents with mass percent should 89%��100%. The screen protection panel of electron device with display equipment obtained by the aforementioned chilled glass obtained or the glass cover of electronics outer cover. With the electron device of display equipment can be mobile phone, computer, PAD, TV, with the receiving set of display screen or stereo set, or the robot etc. with display equipment, electronics outer cover can be shield cap of use for laboratory etc.

Compared with prior art, the invention has the beneficial effects as follows:

What 1, the present invention can remove surface layer of glass oozes tin layers and tiny crack, and is combined by 2 chemical enhanced techniques with microetch so that glass is greatly improved.

2, the chemical enhanced pretreated technique position difference of the present invention and whole process sequence are different, and the glass properties obtained after glass reinforced also can be different, and the characteristic of the chilled glass obtained all is greatly improved.

Embodiment

The present invention is further illustrated below. Embodiments of the present invention include but not limited to the following example.

Embodiment 1

1, glass carries out edging, chamfering, punching process through essence carving machine;

2, Chemical Pretreatment: glass is positioned in saltpetre fused salt and carries out high temperature pre-treatment, pretreatment temperature is 380 DEG C, and the chemical enhanced time is 30min;

3, ultrasonic cleaning: for washing with at the beginning of the alkali lye of 8-10wt%, scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again;

4, microetch process: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media, and the microetch treatment time is 2��15min, and microetch medium bag is represent with mass percent, HF:1%, H₂SO₄: 3%, HNO₃: 4%, all the other are pure water.

5, chemical intensification treatment: glass being put into saltpetre tempering liquid and carries out chemical enhanced, chemical enhanced temperature is 380 DEG C, and the chemical enhanced time is 4 hours.

Embodiment 2

1, glass carries out edging, chamfering, punching process through essence carving machine;

2, Chemical Pretreatment: glass is positioned in saltpetre fused salt and carries out high temperature pre-treatment, pretreatment temperature is 400 DEG C, and the chemical enhanced time is 2min;

3, ultrasonic cleaning: for washing with at the beginning of the alkali lye of 8-10wt%, scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again;

4, microetch process: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media, and the microetch treatment time is 2��15min, and microetch medium bag is represent with mass percent, HF:5%, H₂SO₄: 4%, all the other are pure water.

5, chemical intensification treatment: glass being put into saltpetre tempering liquid and carries out chemical enhanced, chemical enhanced temperature is 430 DEG C, and the chemical enhanced time is 6 hours.

Embodiment 3

1, glass carries out edging, chamfering, punching process through essence carving machine;

2, Chemical Pretreatment: glass is positioned in saltpetre fused salt and carries out high temperature pre-treatment, pretreatment temperature is 390 DEG C, and the chemical enhanced time is 10min;

3, ultrasonic cleaning: for washing with at the beginning of the alkali lye of 8-10wt%, scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again;

4, microetch process: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media, and the microetch treatment time is 2��15min, and microetch medium bag is represent with mass percent, HF:3%, H₂SO₄: 1%, HNO₃: 2%, all the other are pure water.

5, chemical intensification treatment: glass being put into saltpetre tempering liquid and carries out chemical enhanced, chemical enhanced temperature is 420 DEG C, and the chemical enhanced time is 4 hours.

Embodiment 4

1, glass carries out edging, chamfering, punching process through essence carving machine;

2, ultrasonic cleaning: for washing with at the beginning of the alkali lye of 8-10wt%, scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again;

3, microetch process: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media, and the microetch treatment time is 2��15min, and microetch medium bag is represent with mass percent, HF:5%, H₂SO₄: 4%, HNO₃: 3%, all the other are pure water.

4, Chemical Pretreatment: glass is positioned in saltpetre fused salt and carries out high temperature pre-treatment, pretreatment temperature is 390 DEG C, and the chemical enhanced time is 15min;

5, chemical intensification treatment: glass being put into saltpetre tempering liquid and carries out chemical enhanced, chemical enhanced temperature is 400 DEG C, and the chemical enhanced time is 8 hours.

Embodiment 5

1, glass carries out edging, chamfering, punching process through essence carving machine;

2, ultrasonic cleaning: for washing with at the beginning of the alkali lye of 8-10wt%, scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again;

3, microetch process: glass immersion is sprayed pouring at glass surface in microetch medium or by microetch homogeneous media, and the microetch treatment time is 2��15min, and microetch medium bag is represent with mass percent, HF:2%, H₂SO₄: 3%, HNO₃: 2%, all the other are pure water.

4, Chemical Pretreatment: glass is positioned in saltpetre fused salt and carries out high temperature pre-treatment, pretreatment temperature is 380 DEG C, and the chemical enhanced time is 8min;

5, chemical intensification treatment: glass being put into saltpetre tempering liquid and carries out chemical enhanced, chemical enhanced temperature is 430 DEG C, and the chemical enhanced time is 6 hours.

Embodiment 7

Representing with mass percent, the chilled glass that above-described embodiment obtains comprises following component: SiO₂: 60��65%, Al₂O₃: 11��17%, K₂O:0.2%��6.8%, ZrO₂: 0%��1.8%, SiO simultaneously₂+Al₂O₃+Na₂O+K₂O+MgO+ZrO₂The total amount of+CaO represents with mass percent should 89%��100%. The obtained screen protection panel of electron device with display equipment obtained by the aforementioned chilled glass obtained or the glass cover of electronics outer cover.

The lateral comparison of technical process:

It is quantitative taking the processing parameter of embodiment 1, technical process order converts, obtain 1#(embodiment 1), 2#(technical process: carving machine carries out edging, chamfering, after punching processes, carry out ultrasonic cleaning again, microetch processes, chemical enhanced pre-treatment, chemical intensification treatment), 3#(technical process: essence carving machine edging, chamfering, punching ultrasonic cleaning), 4#(technical process: essence carving machine edging, chamfering, punching ultrasonic cleaning is chemical enhanced), 5#(technical process: ultrasonic cleaning micro etch essence carving machine edging, chamfering, punch chemical enhanced), 6#(technical process: essence carving machine edging, chamfering, punching ultrasonic cleaning microetch is chemical enhanced), after carrying out intensive treatment with the glass of equal amts according to the technical process of 1#-6#, carry out bearing stress, compressive stress layer thickness and falling sphere, the test that angle, face is fallen, test result is such as table 1:

Table 1

As can be seen from the above table, 1# and 2# glass sample after processing method step process of the present invention, its surface strength is greatly improved, performance after tempering is all in higher level, and positioning height 85CM falling sphere 3 Secondary Shocks tested glass slip gradient is less than 5%, positioning height 160CM face falls that 3 tested glass slip gradient even reach 1.5%, 2 tested glass slip gradient are fallen equally also lower than less than 15% in positioning height 50CM angle.

From longitudinal comparison, embodiment 1-embodiment 5 carrying out bearing stress and the test of compressive stress layer thickness, test result is such as table 2:

As can be seen from the above table, the two-sided compressive stress layer one-tenth-value thickness 1/10 of embodiment 1-5 at 30-50 �� m,

Bearing stress value average is between 820-880MPa.

It is embodiments of the invention as mentioned above. The present invention is not limited to above-mentioned enforcement mode, and anyone should

This learns the structure change made under the enlightenment of the present invention, and every have identical or close technical scheme with the present invention, all falls within protection scope of the present invention.

Claims (10)

1. the enhancement method of a high strength protective glass; it is characterized in that: glass is carried out after edging, chamfering, punching process through essence carving machine; carry out ultrasonic cleaning, microetch process, chemical intensification treatment again; also comprising chemical enhanced pre-treatment, described chemical enhanced pre-treatment can after essence carves machine edging, chamfering, punching process, before ultrasonic cleaning or between microetch process and chemical intensification treatment.

2. enhancement method according to claim 1, it is characterised in that: the microetch medium that microetch process uses comprises following component, represents with mass percent, HF:1%��5%, H₂SO₄: 1%��8%, HNO₃: 0%��5%, HF+H simultaneously₂SO₄+HNO₃+ HCL total amount 7%��12%, all the other are pure water.

3. enhancement method according to claim 1, it is characterised in that: the microetch treatment time is 2��15min.

4. enhancement method according to claim 1, it is characterised in that: ultrasonic cleaning is specially and washes at the beginning of the alkali lye with 8-10wt%, and scavenging period is 5 minutes; Washing by 4-6wt% alkali lye essence, scavenging period is 5 minutes again; Using pure water rinsing again, scavenging period is 20��25 minutes, and pure water is 12��18,000,000; After pure water cleans, wide slow moving water-removal is air-dry again.

5. enhancement method according to claim 1, it is characterised in that: chemical enhanced pre-treatment is specially puts into glass tempering liquid and carries out chemical enhanced, and chemical enhanced pretreated strengthening temperature is 380 DEG C��400 DEG C, and the chemical enhanced time is 2��30min.

6. enhancement method according to claim 5, it is characterised in that: chemical enhanced pretreated strengthening temperature is 390 DEG C��400 DEG C, and the chemical enhanced time is 2��10min.

7. enhancement method according to claim 1, it is characterised in that: chemical intensification treatment is specially to be put into glass tempering liquid and carries out chemical enhanced, and chemical enhanced temperature is 380 DEG C��430 DEG C, and the chemical enhanced time is 4��8 hours.

8. the chilled glass that enhancement method as described in claim 1-7 is obtained, it is characterised in that: double-sided glass microetch thickness is 18��25 ��m, and chemically reinforced glass bearing stress is 820��880Mpa, and the compressive stress layer degree of depth is 30��50 ��m.

9. chilled glass according to claim 8, it is characterised in that: represent with mass percent, comprise following component: SiO₂: 60��65%, Al₂O₃: 11��17%, K₂O:0.2%��6.8%, ZrO₂: 0%��1.8%, SiO simultaneously₂+Al₂O₃+Na₂O+K₂O+MgO+ZrO₂The total amount of+CaO represents with mass percent should 89%��100%.

10. the screen protection panel of the electron device with display equipment obtained by the chilled glass of claim 9 or the glass cover of electronics outer cover.