CN101945831A - 玻璃表面改性的方法 - Google Patents
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Abstract
一种通过对玻璃基材的至少一个表面进行改性来改善玻璃的化学稳定性的方法。该改性方法利用具有小于1000nm的平均空气动力学颗粒直径的结晶金属氧化物颗粒,所述颗粒至少部分嵌入在玻璃表面上和玻璃表面内。一种用于在玻璃表面上沉积结晶金属氧化物的装置。
Description
发明背景
技术领域
本发明涉及一种通过对玻璃基材表面进行改性来改善玻璃的化学稳定性的方法。优选地,在玻璃制造期间或在玻璃加工如玻璃钢化期间进行该表面改性。通过至少部分嵌入玻璃的结晶氧化铝颗粒来改善玻璃的化学稳定性。优选通过改性的液体火焰喷射方法来进行包含铝的颗粒的沉积。
背景技术说明
氧化铝(Al2O3)涂层被用于各种用途,例如光学器件和电子器件。氧化铝涂层是耐擦伤性的,且其用于各种基材上例如金属、半导体和玻璃基材上。使用各种涂覆方法来沉积氧化铝涂层,包括化学气相沉积(CVD)、喷射热解和溅射。
已知,可以通过向玻璃配合料中添加氧化铝或氧化锆来改善玻璃的化学稳定性。但是,配合料的熔点同时需要提高,为了保持玻璃熔体所需的粘度,这将极大提高玻璃的生产成本。
使用常压CVD法来在玻璃带上产生涂层是公知的方法。使用各种前体来在玻璃带上制备氧化铝涂层,如WO 2005/087678 A1,Pilkington North America Inc.,2005年9月22日所述。该出版物记载了在玻璃上制备Al2O3涂层。这样的涂层没有使玻璃基材表面改性,而只是玻璃上的单独涂层。涂层的粘附力以及尤其是因例如环境影响所致的粘附力随时间的变化对于玻璃产品的化学稳定性是个巨大的挑战。
US 3,762,808,Pilkington Brothers Ltd.,2.10,1973记载了在浮法工艺中改善玻璃性质的方法。玻璃的表面特性例如浮法玻璃的色调、透光性和排热特性是通过如下方式改善的:使两种金属以所需比例从熔融合金电解本体迁移到玻璃表面内,该熔融合金保持与热玻璃表面接触。需要熔融金属使得该方法在浮法工艺中变得复杂,且在玻璃加工中成为不可能。
现有技术的问题在于其未提供改善玻璃的化学稳定性且可结合到玻璃制造过程(例如浮法工艺或铸造工艺)中或结合到玻璃加工生产线(例如玻璃钢化)中的方法。
发明概述
本发明的主要目的是引入一种通过对玻璃基材的至少一个表面进行改性用来改善玻璃的化学稳定性的方法。该改性方法利用了具有小于1000nm的平均空气动力学颗粒直径的结晶金属氧化物颗粒,所述颗粒至少部分嵌入在玻璃表面上且嵌入玻璃表面中。
在本发明的一个实施方案中,将至少一个玻璃基材表面加热到高于550℃的温度。将包含前体金属M的颗粒沉积在玻璃基材的至少一个表面上,且通过热处理使沉积的颗粒的至少一部分转化成包含结晶金属氧化物MxOy(c)的颗粒。在本发明的另一实施方案中,将玻璃基材的至少一个表面加热到高于550℃的温度。具有小于1000nm的平均空气动力学颗粒直径的结晶金属氧化物颗粒MxOy(c)形成且沉积到玻璃基材的至少一个表面上,其中该表面的温度高于550℃,且包含所述颗粒MxOy(c)的气溶胶的温度高于玻璃表面的温度。优选地,通过气体到颗粒的转化制备所述颗粒。颗粒的尺寸优选小于1000nm,更优选小于100nm且最优选小于50nm。
金属优选为铝或锆。氧化铝(Al2O3)颗粒优选为α-Al2O3颗粒,且其优选通过热处理过程转化为γ-Al2O3颗粒。氧化锆颗粒优选是四方或单斜的。
本发明的另一目的是引入通过对玻璃基材(8)的至少一个表面(9)进行改性来改善玻璃的化学稳定性的装置。该装置包含本体(1)、连接至本体(1)的液体火焰喷枪(2),且还包含雾化器(11)、用于将至少一种液态前体供给喷枪(2)的导管(5)、和用于产生火焰(6)的部件(12)。以使得基本在表面(9)上的火焰(6)的温度高于表面(9)的温度的方式设置火焰(6)和玻璃表面(9)之间的距离。在优选实施方案中,基本在表面(9)上的火焰(6)的温度为至少650℃。
附图简要说明
在下文中,将参照所附原理图来更详细地说明本发明,其中
图1显示了本发明装置的示意图。
为简明计,该图仅显示了对于理解本发明所必需的细节。从图中省略了对于理解本发明非必需且对于本领域技术人员是显而易见的结构和细节,以便强调本发明的特征。
优选实施方式的详细说明
图1在原理上显示了使用改进的液体火焰喷射装置2用于通过本发明的方法对玻璃基材8的至少一个表面9进行改性。至少一个液体火焰喷枪2连接至本体1。该装置包含部件11,用于调节喷枪2和玻璃基材表面9之间的距离。对距离进行调节使得在表面9上的火焰6的温度高于表面9的温度。可以通过经由导管3和4分别供入到液体火焰喷射装置2的燃料和氧化性气体的量来调节火焰6的温度。还可以通过选择燃料气体和氧化性气体来调节火焰6的温度。对于高的火焰6的温度,优选的混合物是氢和氧,对于较低的火焰6的温度,可用空气取代氧且用烃取代氢。通过导管5将液态前体供入枪2中。前体可以例如是金属硝酸盐的溶液。在铝的情形中,液态前体优选为溶于甲醇中的硝酸铝,Al(NO3)3·9H2O。硝酸铝∶甲醇的比率以重量计优选为1∶10-1∶100,更优选约1∶30。流向单一枪2的前体流速优选为1-100毫升/分钟,最优选约10毫升/分钟。通过导管3供给氢气。对于单一枪2,典型的质量流量为5-50升/分钟,优选约30升/分钟。通过导管4供给氧气。对于单一枪2,典型质量流量为2-30升/分钟,优选约15升/分钟。氢气和氧气流经部件12用于产生火焰6,并引发火焰6。通过雾化器11将液态前体供入火焰6,该雾化器11将液态前体转变为小液滴。液滴和前体金属在火焰6中蒸发,且通过气体到颗粒的转化而形成亚微米颗粒7。使用所述铝前体,形成了γ-Al2O3颗粒7。颗粒7的平均空气动力学直径优选小于1000nm,更优选小于100nm,且最优选小于50nm,该尺寸如此小,使得颗粒7不会对玻璃表面9产生显著的光学影响。已发现,至少部分嵌入玻璃表面层9的γ-Al2O3颗粒10可通过在500-750℃温度下的热处理转化为α-Al2O3颗粒。根据玻璃基材8的温度,且更精确地根据玻璃表面层9的温度,前体金属的较小或较大部分可从金属氧化物颗粒7溶入表面层2中。这降低了结晶金属氧化物颗粒11的平均直径,其对于玻璃基材8的光学品质是有利的。在本发明的一个实施方案中,对火焰6和基材表面9之间的距离进行调节,使得在表面9上的火焰6的温度高于表面9的温度。优选地,在表面9上的火焰6的温度为至少650℃,且更优选至少750℃。
还可以调节液体雾化和火焰6的温度使得颗粒7不通过气体到颗粒的转化途径而是通过喷雾干燥来形成。该机制产生了显著较大的颗粒,其具有约1000nm的典型直径。这些颗粒可沉积于表面9上,且通过在500-750℃的热处理将其转变为结晶颗粒。这样的热处理过程可以有利地在浮法玻璃制造过程或在玻璃铸造过程中进行,这对于本领域技术人员是公知的方法。
硝酸锆ZrO(NO3)2是用于制备结晶ZrO2的优选前体。ZrO(NO3)2可以从例如Zr(OH2)CO3粉末制得。浓硝酸可用来溶解粉末,且因而去离子水(H2O)和乙醇可用来获得液态前体。在火焰中,前体蒸发并制得结晶ZrO2。通常,能够鉴别出ZrO2的亚稳的四方相和单斜相两者。认为亚稳相可在较小的颗粒7中占优。
可以根据本发明的精神产生多种实施方案。因此,上述实施例不得理解为对本发明的限制,而是本发明的实施方案可以在本文权利要求所述的发明特征的范围内自由变化。
Claims (10)
1.通过对玻璃基材的至少一个表面进行改性来改善玻璃的化学稳定性的方法,包含至少部分地将结晶金属氧化物MxOy(c)颗粒嵌入在玻璃表面上和玻璃表面内,所述颗粒具有小于1000nm的平均空气动力学颗粒直径。
2.权利要求1的方法,包含:
a.将玻璃基材的至少一个表面加热到高于550℃的温度;
b.在玻璃基材的至少一个表面上沉积包含前体金属M的颗粒;和
c.热处理过程,其足以将包含金属M的沉积颗粒的至少一部分转化为包含结晶金属氧化物MxOy(c)的颗粒。
3.权利要求1的方法,包含:
a.形成结晶金属氧化物MxOy(c)颗粒,其具有小于1000nm的平均空气动力学颗粒直径;及
b.将所述结晶MxOy(c)颗粒沉积到玻璃基材的至少一个表面上,其中所述表面的温度高于550℃,且含有所述颗粒的气溶胶的温度高于玻璃表面的温度。
4.权利要求1-3中任一项的方法,其特征在于,金属是铝。
5.权利要求1-3中任一项的方法,其特征在于,金属是锆。
6.权利要求4的方法,其特征在于,氧化铝Al2O3颗粒是γ-Al2O3颗粒。
7.权利要求6的方法,其还包含足以将至少部分沉积的γ-Al2O3颗粒转化为α-Al2O3颗粒的热处理过程。
8.权利要求1-7中任一项的方法,包含通过气体到颗粒的转化制备颗粒。
9.用于通过对玻璃基材(8)的至少一个表面(9)进行改性来改善玻璃的化学稳定性的装置,包括本体(1)、连接至本体(1)的液体火焰喷枪(2),且还包括雾化器(11)、用于将至少一种液态前体供给喷枪(2)的导管(5)和用于产生火焰(6)的部件(12),其特征在于,以使得基本在表面(9)上的火焰(6)的温度高于表面(9)的温度的方式设置火焰(6)和玻璃表面(9)之间的距离。
10.权利要求9的装置,其特征在于,基本在表面(9)上的火焰(6)的温度为至少650℃。
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FI20080128A FI122879B (fi) | 2008-02-18 | 2008-02-18 | Menetelmä lasin pinnan muokkaamiseksi |
FI20080128 | 2008-02-18 | ||
PCT/FI2009/000026 WO2009103842A1 (en) | 2008-02-18 | 2009-02-17 | Glass surface modification process |
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CN101945831A true CN101945831A (zh) | 2011-01-12 |
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CN2009801050679A Pending CN101945831A (zh) | 2008-02-18 | 2009-02-17 | 玻璃表面改性的方法 |
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US (1) | US20110041556A1 (zh) |
EP (1) | EP2250134A4 (zh) |
CN (1) | CN101945831A (zh) |
EA (1) | EA017910B1 (zh) |
FI (1) | FI122879B (zh) |
WO (1) | WO2009103842A1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107735377A (zh) * | 2015-07-08 | 2018-02-23 | 旭硝子株式会社 | 功能性玻璃物品及其制造方法 |
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FI20061014A0 (fi) * | 2006-11-17 | 2006-11-17 | Beneq Oy | Diffuusiopinnoitusmenetelmä |
WO2011036155A2 (en) * | 2009-09-25 | 2011-03-31 | Agc Glass Europe | Decorative glass article |
US9988304B2 (en) * | 2011-09-02 | 2018-06-05 | Guardian Glass, LLC | Method of strengthening glass by plasma induced ion exchanges in connection with tin baths, and articles made according to the same |
US11213848B2 (en) * | 2015-12-11 | 2022-01-04 | Vitro Flat Glass Llc | Nanoparticle coater |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2007110482A1 (en) * | 2006-03-27 | 2007-10-04 | Beneq Oy | A method for producing functional glass surfaces by changing the composition of the original surface |
Family Cites Families (8)
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US3762808A (en) * | 1970-05-22 | 1973-10-02 | A Sandmeier | Data reproduction apparatus |
US5637353A (en) * | 1990-09-27 | 1997-06-10 | Monsanto Company | Abrasion wear resistant coated substrate product |
US6919054B2 (en) * | 2002-04-10 | 2005-07-19 | Neophotonics Corporation | Reactant nozzles within flowing reactors |
DE10219812A1 (de) * | 2002-05-02 | 2003-11-13 | Univ Dresden Tech | Bauteile mit kristallinen Beschichtungen des Systems Aluminiumoxid/Siliziumoxid und Verfahren zu deren Herstellung |
AU2003296882A1 (en) * | 2002-07-19 | 2004-05-04 | Ppg Industries Ohio, Inc. | Article having nano-scaled structures and a process for making such article |
FI20061014A0 (fi) * | 2006-11-17 | 2006-11-17 | Beneq Oy | Diffuusiopinnoitusmenetelmä |
FI123798B (fi) * | 2007-04-23 | 2013-10-31 | Beneq Oy | Energiansäästölasi ja menetelmä sen valmistamiseksi |
CN101755074A (zh) * | 2007-07-20 | 2010-06-23 | 国立大学法人长冈技术科学大学 | 氮化物膜的沉积方法及沉积装置 |
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2008
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2009
- 2009-02-17 US US12/811,714 patent/US20110041556A1/en not_active Abandoned
- 2009-02-17 CN CN2009801050679A patent/CN101945831A/zh active Pending
- 2009-02-17 EP EP09712653A patent/EP2250134A4/en not_active Withdrawn
- 2009-02-17 EA EA201070946A patent/EA017910B1/ru not_active IP Right Cessation
- 2009-02-17 WO PCT/FI2009/000026 patent/WO2009103842A1/en active Application Filing
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2007110482A1 (en) * | 2006-03-27 | 2007-10-04 | Beneq Oy | A method for producing functional glass surfaces by changing the composition of the original surface |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107735377A (zh) * | 2015-07-08 | 2018-02-23 | 旭硝子株式会社 | 功能性玻璃物品及其制造方法 |
Also Published As
Publication number | Publication date |
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EA201070946A1 (ru) | 2011-02-28 |
FI20080128A (fi) | 2009-08-19 |
EP2250134A1 (en) | 2010-11-17 |
FI20080128A0 (fi) | 2008-02-18 |
EA017910B1 (ru) | 2013-04-30 |
EP2250134A4 (en) | 2011-04-27 |
US20110041556A1 (en) | 2011-02-24 |
FI122879B (fi) | 2012-08-15 |
WO2009103842A1 (en) | 2009-08-27 |
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