CN1369449A - 一种玻璃综合增强方法 - Google Patents
一种玻璃综合增强方法 Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000005728 strengthening Methods 0.000 title abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000005357 flat glass Substances 0.000 claims abstract description 6
- 238000004381 surface treatment Methods 0.000 claims abstract description 6
- 238000005496 tempering Methods 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 claims description 3
- 239000011241 protective layer Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- 239000011253 protective coating Substances 0.000 claims 2
- 239000002904 solvent Substances 0.000 claims 2
- 229910014458 Ca-Si Inorganic materials 0.000 claims 1
- 229910017855 NH 4 F Inorganic materials 0.000 claims 1
- 239000003973 paint Substances 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 235000011194 food seasoning agent Nutrition 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000002950 deficient Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910000919 Air-hardening tool steel Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007603 infrared drying Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/31—Pre-treatment
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
采用化学钢化与表面处理、表面保护相结合,来增强平板玻璃或玻璃制品的方法。它包括玻璃表面预处理、化学钢化、表面后处理、表面保护四个过程,可以将普通平板玻璃的弯曲强度提高到1000MPa以上。
Description
本发明阐述一种能够大幅度提高玻璃弯曲强度的增强方法，它的特征是采用化学钢化、化学腐蚀和涂层保护相结合的综合途径，来增强玻璃的韧性和强度。
普通平板玻璃实际强度只有50～80Mpa左右，而玻璃的理论强度可达到10000～20000Mpa。这之间2～3个数量级的巨大差异，主要是由于玻璃内、外部的缺陷造成的，其中表面缺陷特别是裂纹的影响更为显著。目前，玻璃增强主要采取在表面造成压缩应力层的方法，如风钢化、液体钢化、固体微粒钢化、化学钢化等，已取得广泛的实际应用。表面压应力增强方法的局限在于表层产生压缩应力的同时，在玻璃内部产生相应的与之平衡的张应力，因而，引入的压应力值不能过高，增强效果受到限制。依据工艺方法的不同，玻璃弯曲强度一般可提高到150～450MPa之间；化学腐蚀也是玻璃增强的一种方法，它是通过化学处理，去除玻璃表面缺陷层，使表面趋于“无缺陷”的理想状态，从而恢复玻璃固有的高强度。化学腐蚀存在的主要问题，一是腐蚀过程经常引起玻璃表面光学性能的降低；二是恢复的强度不能持久，衰减十分严重。
为提高玻璃强度，前人在综合增强方面做过一些探索。US3287200，采用风钢化结合化学钢化的方式。风钢化形成的压缩应力层厚但表面应力小；化学钢化的表面应力层薄但表面应力大。该专利希望能够综合两种钢化增强方法的优点，形成表面应力大并且应力层厚的制品。但实际上，该专利的可行性存在问题，实践表明，在450℃的化学钢化温度下，风钢化产生的应力会迅速松弛，失去增强效果，无法形成复合应力层。
用化学溶液特别是酸溶液如HF酸腐蚀增强玻璃的案例更多的见于实验室结果，实际商业应用很少。主要原因是表面腐蚀增强虽然暂时都能得到较高的强度值，但玻璃表面由于环境作用产生缺陷后，强度会急剧丧失，失去增强效果。即便在玻璃腐蚀后用有机涂层形成保护，这种单纯依靠表面增强的结构仍然具有很大的脆弱性，强度值分散程度较大。RU649672提供一种用HF酸和熔盐先后腐蚀、再进行化学钢化的综合增强方法，可以提高增强后制品强度的高温稳定性。从数据看，其强度仅能提高3～4倍，与单纯化学钢化的效果相差不大。
本专利更加完善地提出表面预处理、钢化、表面后处理、表面保护的综合增强方法。其目的就是稳定地大幅度提高并保持玻璃(制品)的强度。
本发明的具体描述如下：
玻璃的预处理。目的是为了在钢化前最大程度去除玻璃表面的微裂纹、划伤等微观宏观缺陷，提高玻璃强度，并且增加表面离子可交换性，促进化学钢化。预处理液的适宜组分为：HF酸浓度6.0N～8.5N，磷酸和硫酸分别占总溶液总重的5～8％，起缓冲作用的NH4F加入量8～10％。表面处理时间是室温下5～15分钟，表面去除厚度50～90微米。以下是最佳参数：
表1
| HF酸浓度 | 磷酸浓度 | 硫酸浓度 | NH4F浓度 | 表面处理时间 | 表面去除厚度 |
| 7.2N | 5％ | 8％ | 8.5％ | 12分钟 | 80微米 |
化学钢化。表面预处理后的制品用去离子水洗净，在无尘的洁净环境下自然干燥后进行钢化增强。化学钢化的最佳工艺参数控制为：交换温度420～480℃，交换时间6～30小时。推荐参数为交换温度450℃，交换时间20小时。
表面后处理。目的是在已形成应力层的玻璃表面进一步消除缺陷。后处理液可以与预处理液成分相同，但处理时间要短。表面腐蚀深度不能超过钢化应力层的厚度。最佳的条件是在室温下处理1～2分钟，腐蚀深度5～15微米。表面后处理后的制品用无水乙醇或异丙醇脱水10～20分钟，在无尘的洁净环境下自然干燥。
表面保护。表面保护的目的是保持酸液后处理的效果，防止在外界影响下制品强度的下降。形成保护层的材料为有机涂料，特别推荐有机硅改性丙烯酸、改性环氧树脂和PVB醇溶液。保护层的施加方法为喷涂或浸渍。涂层后的制品在红外干燥箱于60～100℃下干燥。
本发明与已知的玻璃增强或综合增强方法相比，显著优点是解决了增强后的玻璃制品强度衰减问题，降低了强度分散性，能够大幅度提高普通平板玻璃或制品的强度，玻璃双环抗弯强度可以稳定地提高到800～1000Mpa，最大达到1400Mpa。
实施例：
100×100×3mm浮法玻璃样品，成分如下：
表2
| SiO2 | Al2O3 | CaO | MgO | Na2O | K2O |
| 72 | 1.8 | 7.2 | 4.0 | 14.5 | 0.5 |
用去离子水清洗干净自然干燥，在环境温度25℃，湿度40％条件下，在表1所示地腐蚀液中处理12分钟，其中前10分钟用洁净气体鼓泡搅拌，后2分钟停止搅拌。处理后的样品在25℃的洁净环境自然干燥1小时，之后在450℃的KNO3熔盐中离子交换增强(化学钢化)20小时。钢化后的制品用清水和去离子水洗净，在同样成分的处理液中处理1分钟。处理后的样品在25℃的洁净环境自然干燥0.5小时，之后用有机硅改性丙烯酸液浸涂两次。涂层后的制品在红外干燥箱80℃下干燥24小时。
干燥后的样品用WD-5A万能材料试验机采用双环抗弯方法测试。原片玻璃及增强后的玻璃强度测试结果分别见表3和表4：
表3
| 样品编号 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 平均强度 |
| 强度MPa | 80 | 77 | 85 | 92 | 71 | 104 | 124 | 65 | 73 | 62 | 83 |
表4
| 样品编号 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 平均强度 |
| 强度MPa | 956 | 1031 | 982 | 1153 | 947 | 978 | 1205 | 994 | 1298 | 1194 | 1058 |
Claims (8)
1、一种大幅度提高玻璃强度的增强方法，该方法包括以下步骤：
(a)用腐蚀性溶液对玻璃进行表面处理；
(b)对处理过的玻璃进行化学钢化增强；
(c)对化学钢化后的玻璃进行表面后处理；
(d)在处理后玻璃表面形成保护层。
2、按权利要求1的方法，玻璃是指普通Na-Ca-Si平板玻璃或玻璃制品。
3、按权利要求1的方法，其中步骤(a)和步骤(c)所指表面处理液是以HF酸为主的对玻璃表面具有腐蚀性的液体。
4、按权利要求1的方法，玻璃在表面处理后要经过一个溶剂脱水过程。
5、按权利要求1的方法，其中步骤(d)是指用有机硅改性丙烯酸涂料在玻璃表面形成保护涂层。
6、按权利要求3的方法，处理液中的其它组分为磷酸、盐酸和NH4F。
7、按权利要求4的方法，脱水溶剂为无水乙醇或异丙醇。
8、按权利要求5的方法，有机保护涂层是在新形成的无损伤的玻璃表面形成。
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| CN1369449A true CN1369449A (zh) | 2002-09-18 |
| CN1161298C CN1161298C (zh) | 2004-08-11 |
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Cited By (35)
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| CN100386276C (zh) * | 2005-11-04 | 2008-05-07 | 深圳创维－Rgb电子有限公司 | 一种镜画视窗薄钢化玻璃的制作方法 |
| CN101928110A (zh) * | 2008-12-26 | 2010-12-29 | Hoya株式会社 | 玻璃基材及其制造方法 |
| CN102424530A (zh) * | 2011-09-02 | 2012-04-25 | 信利光电(汕尾)有限公司 | 提高钢化玻璃切割后抗压强度的方法 |
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| CN102791646A (zh) * | 2010-02-02 | 2012-11-21 | 苹果公司 | 用于便携式电子设备的盖体的增强的化学强化玻璃 |
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| CN103508674A (zh) * | 2012-06-27 | 2014-01-15 | 成都光明光电股份有限公司 | 玻璃增强方法 |
| CN103508680A (zh) * | 2012-06-18 | 2014-01-15 | 胜华科技股份有限公司 | 玻璃强化涂料及具有玻璃强化涂料的强化玻璃切割件 |
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-
2002
- 2002-03-26 CN CNB021162484A patent/CN1161298C/zh not_active Expired - Lifetime
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