CN105366924A - Glass annealing method and application thereof - Google Patents
Glass annealing method and application thereof Download PDFInfo
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- CN105366924A CN105366924A CN201410440644.2A CN201410440644A CN105366924A CN 105366924 A CN105366924 A CN 105366924A CN 201410440644 A CN201410440644 A CN 201410440644A CN 105366924 A CN105366924 A CN 105366924A
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Abstract
The invention discloses a glass annealing method and application thereof, and particularly relates to a float-produced glass annealing method and application thereof. The glass annealing method comprises the steps that the temperature of glass is increased to T1 DEG C, and T1 is the glass-transition temperature Tg or temperature 10 DEG C-30 DEG C below the Tg when the glass is prepared; after heat preservation is performed on the glass for 1-20 hours at T1 DEG C, the temperature is lowered to T2 DEG C at the constant speed, a temperature difference value of the T1 and the T2 serves as a temperature lowering range, and the temperature lowering range is 60 DEG C-120 DEG C; in the temperature lowering range, the temperature lowering rate of the temperature of the glass is kept at minus 60 DEG C/h-minus 2 DEG C/h. According to the glass prepared through the glass annealing method, the stress distribution is more uniform, surface stress values are determined according to a surface stress method, and the dispersion coefficients of the surface stress values can be controlled within 0.05 after statistical calculation is performed.
Description
Technical field
The present invention relates to a kind of glass annealing method and application thereof, particularly relate to a kind of glass annealing method and application thereof of float process.
Background technology
Chemically reinforced glass to be applicable to chemical enhanced glass, such as Na
2o-Al
2o
3-SiO
2the glass of system, is immersed in the exchange containing carrying out Na-K ion in potassium ion solution, such as KNO
3in solution, thus obtain the chilled glass of surface high pressure stress.Glass is after strengthening, and the hardness of glass, resistance to marring, shock resistance will be significantly improved.
Although this type of technological process existing can be carried out strengthening to glass and be improved its tempering performance, usually in process of production, because of the infusibility Al of high-content in component
2o
3the glass ununiformity caused and the stress inhomogeneous caused in annealing process because of float glass make the intensity of itself be starkly lower than theoretical strength, glass tempering performance when therefore the tempering performance of gained glass is starkly lower than desired design after actual strengthening.
Summary of the invention
The applicant finds through large quantifier elimination, a problem is there is at present in this type of technological process, the stress distribution ununiformity that the ununiformity produced in large-scale production process because of glass and glass produce when cooling fast causes the difference of glass reinforced effect to exist always, shows that the discreteness of glass reinforced rear tempering performance is larger.Due to the discreteness of tempering performance segment glass can be made to strengthen after lower than expection tempering performance, thus the quality of glass is reduced.
In view of this, the invention provides a kind of glass annealing method and application thereof, the glass strain distribution that described glass annealing method produces is comparatively even, and surface stress value measures according to surface stress method, and after statistical computation, its coefficient of dispersion can be controlled within 0.05.
For solving above technical problem, the technical scheme of first aspect provided by the invention is a kind of glass annealing method, comprises the following steps:
Glass is warming up to T1 DEG C, glass transition temperature Tg when T1 is glass preparation or below Tg 10 ~ 30 DEG C; Glass is incubated when T1 DEG C that to carry out temperature-reduction at constant speed to the temperature gap of T2 DEG C, T1 and T2 after 1-20 hour be between cooling area, is 60-120 DEG C between described cooling area; In in described cooling area, glass keeps the rate of temperature fall of own temperature to be-60 DEG C/h ~-2 DEG C/h.
Preferably, glass, after temperature-reduction at constant speed, adopts Temperature fall or forced cooling either type.
Preferably, in described cooling area, glass keeps the rate of temperature fall of own temperature to be-30 DEG C/h ~-7.5 DEG C/h.
Preferably, in described cooling area, glass keeps the rate of temperature fall of own temperature to be-15 DEG C/h ~-7.5 DEG C/h.
Preferably, described glass is Na
2o-Al
2o
3-SiO
2the glass of system, glass carries out temperature-reduction at constant speed to T2 DEG C after being incubated 10-15 hour when T1 DEG C.
The application also provides the technical scheme of second aspect and aforementioned arbitrary described glass annealing method improving the application in glass tempering performance, utilizes the glass obtained by aforementioned arbitrary glass annealing method to carry out chemical enhanced.
Preferably, the described chemical enhanced exchange for glass being immersed in containing carrying out Na-K ion in potassium ion solution.
Preferably, described glass is Na
2o-Al
2o
3-SiO
2the glass of system, glass carries out temperature-reduction at constant speed to T2 DEG C after being incubated 10-15 hour when T1 DEG C.
Preferably, described is KNO containing potassium ion solution
3solution.
Compared with prior art, it is described in detail as follows the application:
Described in the application, glass annealing method mainly adopts following steps:
Glass is warming up to T1 DEG C, glass transition temperature Tg when T1 is glass preparation or below Tg 10 ~ 30 DEG C; Glass is incubated when T1 DEG C that to carry out temperature-reduction at constant speed to the temperature gap of T2 DEG C, T1 and T2 after 1-20 hour be between cooling area, is 60-120 DEG C between described cooling area; In in described cooling area, glass keeps the rate of temperature fall of own temperature to be-60 DEG C/h ~-2 DEG C/h.
The applicant is found by large quantifier elimination, above-mentionedly gained glass carried out above-mentioned second annealing mode by adopting or aforesaid way is applied in the annealing process of glass, to adopt between above-mentioned specific heat preservation zone, between specific temperature-reduction at constant speed speed and cooling area, thus glass that Uniformity of Stress is improved can be obtained or directly obtain the comparatively uniform glass of stress distribution.The application's gained glass simultaneously can effectively after its strengthening, and the discreteness of its tempering performance obviously improves, thus the tempering performance of glass can closer to the set(ting)value of expection.By to adopting common annealing mode and the glass that adopts mode described in the application to carry out second annealing on common annealing mode basis to measure, find that the tempering performance of the glass adopting the application's mode improves more than 10%, after strengthening, glass tempering performance profile discreteness then reduces by more than 50%.
Accompanying drawing explanation
Fig. 1 is the application's embodiment glass annealing method;
Fig. 2 be in embodiment 2 glass strengthen at different conditions after surface stress value variation diagram;
Fig. 3 be in embodiment 2 glass strengthen at different conditions after stressor layers change in depth figure.
embodiment
The application's glass annealing method, comprises the following steps,
Glass is warming up to T1 DEG C, glass transition temperature Tg when T1 is glass preparation or below Tg 10 ~ 30 DEG C; Glass soaking time when T1 DEG C is that to carry out temperature-reduction at constant speed after △ H=1-20 hour to the temperature gap △ T of T2 DEG C, T1 and T2 be between cooling area, is 60-120 DEG C between described cooling area; In in described cooling area, glass keeps the rate of temperature fall △ d of own temperature be-60 DEG C/h ~-2 DEG C/h, reference Fig. 1.
In order to make those skilled in the art understand technical scheme of the present invention better, below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1---different glass kind is annealed
Aforementioned annealing way is adopted to carry out second annealing to different glass kinds, and carry out chemical enhanced respectively with the different glass kind adopting existing annealing way directly to obtain, the strengthening temperature adopted time chemical enhanced, enhanced time are all identical, are respectively 430 DEG C and 6h; When adopting the application's method for annealing to carry out second annealing to glass, adopting different temperature-reduction at constant speed speed to different glass kinds respectively, identical warming temperature and temperature holding time, is 60-120 DEG C between cooling area.
Gained glass detects following technical indicator, stress and the stressor layers degree of depth adopt FSM-6000 surface stress instrument to test, often kind of sample size at about 20, then according to test result calculations coefficient of dispersion, coefficient of dispersion is calculated as sample standard deviation/sample mean, and acquired results sees the following form.
Table 1---different glass kind annealing determination data
Embodiment 2---same glass kind, different strengthening temperature
Adopt aforementioned annealing way to same glass kind Na
2o-Al
2o
3-SiO
2in system, arbitrary glass kind such as aforementioned MJB5A product carries out second annealing, and carries out chemical enhanced respectively with the glass adopting existing annealing way directly to obtain, and adopts different strengthening temperature, identical enhanced time 6h time chemical enhanced; When adopting the application's method for annealing to carry out second annealing to glass, adopting different temperature-reduction at constant speed speed to glass kind respectively, identical warming temperature and temperature holding time, is 60-120 DEG C between cooling area.
Gained glass detects following technical indicator, and acquired results sees the following form.
Table 2---different strengthening temperature measuring result
Embodiment 3---same glass kind, different warming temperature
Adopt aforementioned annealing way to same glass kind Na
2o-Al
2o
3-SiO
2any one glass kind in system, as aforementioned MJB5A product, carries out second annealing, and carries out chemical enhanced respectively with the glass adopting existing annealing way directly to obtain, and adopts identical strengthening temperature 410 DEG C, enhanced time 6h time chemical enhanced; When adopting the application's method for annealing to carry out second annealing to glass, respectively different temperature-reduction at constant speed speed is adopted to glass kind, different warming temperature (glass transition temperature Tg is 575 DEG C), identical temperature holding time are 60-120 DEG C between cooling area.
Gained glass detects following technical indicator, and acquired results sees the following form.
Table 3---different warming temperature measurement result
Interpretation:
In embodiment 1, the stress value of the annealed rear glass of glass of different varieties increases all to some extent, the coefficient of dispersion of glass then starts to reduce, under different annealing rates, the degree that stress value increases is different with the change of discreteness, and this inspires us can improve annealing rate to reduce costs when meeting the demands.
In embodiment 2, the tempering stress value that different strengthening temperature obtains is different, and in general, within the identical tempering time, tempering temperature is higher, and the stressor layers degree of depth of glass is about dark, and stress value then reduces.The discreteness of the stress value after glass tempering is not obvious with the tempering temperature relation of glass, and the general tempering temperature being applicable to the glass of chemical tempering has a wider interval, coordinates the tempering time can both be met the toughened glass of tempering performance.
In embodiment 3, the holding temperature of different annealing on the impact of tempering performance, in general, when annealing temperature reduces, the time of inside glass structural rearrangement will lengthen, under identical soaking time, when temperature is higher, the degree that inside glass reaches balance will improve.But there is a prerequisite at this, because generation is out of shape by the impact of self gravitation by sheet glass in annealing process, therefore should selects relatively low temperature or prevent glass deformation in the high-temperature time insulation short period in annealing process.The soaking time of sample is 6 hours, and glass all can reach the object improving tempering performance.
Below be only the preferred embodiment of the present invention, it should be pointed out that above-mentioned preferred implementation should not be considered as limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For those skilled in the art, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (9)
1. a glass annealing method, is characterized in that, comprises the following steps:
Glass is warming up to T1 DEG C, glass transition temperature Tg when T1 is glass preparation or below Tg 10 ~ 30 DEG C; Glass is incubated when T1 DEG C that to carry out temperature-reduction at constant speed to the temperature gap of T2 DEG C, T1 and T2 after 1-20 hour be between cooling area, is 60-120 DEG C between described cooling area; In in described cooling area, glass keeps the rate of temperature fall of own temperature to be-60 DEG C/h ~-2 DEG C/h.
2. glass annealing method according to claim 1, is characterized in that: glass, after temperature-reduction at constant speed, adopts Temperature fall or forced cooling either type.
3. glass annealing method according to claim 1, is characterized in that: in described cooling area, glass keeps the rate of temperature fall of own temperature to be-30 DEG C/h ~-7.5 DEG C/h.
4. glass annealing method according to claim 1, is characterized in that: in described cooling area, glass keeps the rate of temperature fall of own temperature to be-15 DEG C/h ~-7.5 DEG C/h.
5. glass annealing method according to claim 1, is characterized in that: described glass is Na
2o-Al
2o
3-SiO
2the glass of system, glass carries out temperature-reduction at constant speed to T2 DEG C after being incubated 10-15 hour when T1 DEG C.
6. the arbitrary described glass annealing method of claim 1-4 is improving the application in glass tempering performance, it is characterized in that: utilize the glass obtained by aforementioned arbitrary glass annealing method to carry out chemical enhanced.
7. application according to claim 6, is characterized in that: the described chemical enhanced exchange for being immersed in by glass containing carrying out Na-K ion in potassium ion solution.
8. application according to claim 7, is characterized in that: described glass is Na
2o-Al
2o
3-SiO
2the glass of system, glass carries out temperature-reduction at constant speed to T2 DEG C after being incubated 10-15 hour when T1 DEG C.
9. application according to claim 8, is characterized in that: described is KNO containing potassium ion solution
3solution.
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|---|---|---|---|
| CN201410440644.2A CN105366924B (en) | 2014-09-01 | 2014-09-01 | Glass method for annealing and its application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410440644.2A CN105366924B (en) | 2014-09-01 | 2014-09-01 | Glass method for annealing and its application |
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| CN105366924B CN105366924B (en) | 2018-09-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618755A (en) * | 2004-11-02 | 2005-05-25 | 中国科学院上海光学精密机械研究所 | Oxychloro bismuth germanate glass and its preparation method |
| CN1927752A (en) * | 2006-09-27 | 2007-03-14 | 中国科学院上海光学精密机械研究所 | Infrared transparent fluozirconate microcrystalline glass and preparation method thereof |
| CN101597134A (en) * | 2009-07-29 | 2009-12-09 | 成都光明光电股份有限公司 | Glass fine annealing device and annealing process thereof |
| CN103648996A (en) * | 2011-07-01 | 2014-03-19 | 康宁股份有限公司 | Ion exchangeable glass with high compressive stress |
-
2014
- 2014-09-01 CN CN201410440644.2A patent/CN105366924B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618755A (en) * | 2004-11-02 | 2005-05-25 | 中国科学院上海光学精密机械研究所 | Oxychloro bismuth germanate glass and its preparation method |
| CN1927752A (en) * | 2006-09-27 | 2007-03-14 | 中国科学院上海光学精密机械研究所 | Infrared transparent fluozirconate microcrystalline glass and preparation method thereof |
| CN101597134A (en) * | 2009-07-29 | 2009-12-09 | 成都光明光电股份有限公司 | Glass fine annealing device and annealing process thereof |
| CN103648996A (en) * | 2011-07-01 | 2014-03-19 | 康宁股份有限公司 | Ion exchangeable glass with high compressive stress |
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