CN110291159A - 包含疏水硅烷的涂料和制品 - Google Patents
包含疏水硅烷的涂料和制品 Download PDFInfo
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- CN110291159A CN110291159A CN201880011472.3A CN201880011472A CN110291159A CN 110291159 A CN110291159 A CN 110291159A CN 201880011472 A CN201880011472 A CN 201880011472A CN 110291159 A CN110291159 A CN 110291159A
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- China
- Prior art keywords
- product
- silicrete
- silane compound
- superficial layer
- weight
- Prior art date
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- 229910000077 silane Inorganic materials 0.000 title claims abstract description 83
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims description 39
- 230000002209 hydrophobic effect Effects 0.000 title abstract description 11
- 238000000576 coating method Methods 0.000 title description 24
- 239000011248 coating agent Substances 0.000 title description 22
- -1 silane compound Chemical class 0.000 claims abstract description 91
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 36
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 24
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008199 coating composition Substances 0.000 claims abstract description 9
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 8
- 239000010432 diamond Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims description 55
- 239000000203 mixture Substances 0.000 claims description 45
- 125000000217 alkyl group Chemical group 0.000 claims description 19
- 229920000620 organic polymer Polymers 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 15
- 239000007795 chemical reaction product Substances 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
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- 239000010703 silicon Substances 0.000 description 12
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- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- 125000003710 aryl alkyl group Chemical group 0.000 description 3
- 125000002102 aryl alkyloxo group Chemical group 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000006184 cosolvent Substances 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 3
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- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 3
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
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- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 3
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 2
- PUGOMSLRUSTQGV-UHFFFAOYSA-N 2,3-di(prop-2-enoyloxy)propyl prop-2-enoate Chemical compound C=CC(=O)OCC(OC(=O)C=C)COC(=O)C=C PUGOMSLRUSTQGV-UHFFFAOYSA-N 0.000 description 2
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- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 description 2
- NLGDWWCZQDIASO-UHFFFAOYSA-N 2-hydroxy-1-(7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-yl)-2-phenylethanone Chemical compound OC(C(=O)c1cccc2Oc12)c1ccccc1 NLGDWWCZQDIASO-UHFFFAOYSA-N 0.000 description 2
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- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10018—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising only one glass sheet
- B32B17/10027—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising only one glass sheet the glass sheet not being an outer layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/082—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising vinyl resins; comprising acrylic resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/09—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyesters
-
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Abstract
本发明描述了包括表面层的制品,该表面层包含至少一种键合到硅质层诸如钻石样玻璃的长疏水性硅烷化合物(C8‑C36)。在一个实施方案中,该硅质层具有不大于10%的孔隙率和不大于1微米的厚度。在另一个实施方案中,该硅质层包含10原子%至50原子%的碳,并且该制品还包含有机聚合物基底构件或硬质涂层。还描述了包含至少一种C8‑C17烃硅烷化合物和至少一种C18‑C36氢化硅烷化合物的涂料组合物。
Description
发明内容
一直需要表现出改善的可擦除性的表面,诸如用干纸巾清洁移除耐久性记号笔油墨的能力。
在一些有利的实施方案中,表面还表现出对多种书写工具(包括耐久性记号笔)良好的油墨接受性,并且适用于干擦板的书写表面。在其他实施方案中,表面表现出低剥离粘附力并且适于用作剥离层。
在一个实施方案中,描述了一种制品,其包含表面层,该表面层包含至少一种键合到硅质层的(例如C8-C36烃)疏水硅烷化合物硅氧烷,该硅质层具有不大于10%的孔隙率和不大于1微米的厚度。
在另一个实施方案中,描述了一种制品,其包含表面层,该表面层包含至少一种键合到硅质层的(例如C8-C36烃)疏水硅烷化合物硅氧烷,该硅质层包含10原子%至50原子%的碳,并且该制品还包括有机聚合物基底构件。
在一些实施方案中,硅质层为钻石样玻璃薄膜层。硅质层通常具有不大于1微米的厚度。
在一些实施方案中,该制品还包括有机聚合物基底构件,例如(例如PET膜)。在一些实施方案中,该制品还包括设置在有机聚合物基底构件和钻石样玻璃层之间的硬质涂层。
在一些实施方案中,该制品为干擦板。耐久性记号笔迹可用干纸巾从表面层擦除。在一些实施方案中,表面层是剥离层。
在另一个实施方案中,描述了一种涂料组合物,其包含至少一种C8-C16烃硅烷化合物和至少一种C18-C36烃硅烷化合物以及任选的有机溶剂。该组合物还可任选地包含其他硅烷化合物。
附图说明
本发明将参考附图进一步进行说明,其中:
图1为示例性实施方案制品的示意图;
图2为另一个示例性实施方案制品的示意图。
这些图未按比例绘制,并且旨在仅为例示性的而非限制性的。
具体实施方式
图1示出了制品10的示例性实施方案,其包括主体构件12,该主体构件具有与硅质层13的前表面16键合的表面层14硅氧烷。在所示的实施方案中,制品10还包括任选的主体构件12,该主体构件通常包括有机聚合物基底构件15。制品10还包括任选的粘合剂层18,以及在主体构件12的背部表面22上任选的可移除的衬里20。
图2示出了制品10的另一个示例性实施方案,其包括主体构件12,该主体构件具有与硅质层13的前表面16键合的表面层14硅氧烷。在所示的实施方案中,制品10还包括任选的主体构件12,该主体构件通常包括有机聚合物基底构件15。硬质涂层17设置在硅质层13和有机聚合物基底构件15之间。制品10还包括任选的粘合剂层18,以及在主体构件12的背部表面22上任选的可移除的衬里20。
在一些实施方案中,基底构件15基本上由包含有机聚合物材料的表面组成或具有包含有机聚合物材料的表面。
有机聚合物材料的示例性示例包括聚酯(例如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二酯(PEN)、聚对苯二甲酸丁二醇酯)、聚烯烃(例如聚丙烯,包括双轴取向聚丙烯(BOPP)、同步双轴取向聚丙烯(S-BOPP)、聚乙烯)、以及乙烯或丙烯共聚物)、三聚氰胺树脂、聚氯乙烯、聚碳酸酯、聚烯丙基二甘醇碳酸酯、聚丙烯酸酯如聚(甲基丙烯酸甲酯)、聚苯乙烯、聚砜、聚醚砜、均聚-环氧聚合物、环氧加成聚合物与聚二胺、聚二硫醇、聚乙烯共聚物、纤维素酯如乙酸酯(例如TAC)和丁酸酯、生物聚合物如聚乳酸基聚合物、以及它们的共混物。
有机聚合物基底构件可任选地还包括附加的有机层或无机层(未示出)。此类附加层可包括玻璃、金属片材、纸材、纸板、针织材料、织物等。
在其他实施方案中,基底构件可包括无机基底,诸如硅质材料(例如玻璃)或金属。
基底构件可以是不透明的或透光的(例如半透明的或透明的)。术语透光性是指透射可见光谱(约400至约700nm波长)内的入射光的至少约85%。基底可被着色。
本文所用的基底构件可根据需要为柔性或非柔性的。
在一些实施方案中,基底构件为自承式的,即尺寸足够稳定以在其移动、使用、或者操作时保持其形状。在一些实施方案中,所述制品以某些方式进一步被支撑,如用加固架、粘附至支撑表面等。
在一些实施方案中,基底构件可具有在其表面上或嵌入其中的图形(例如本领域已知的词语或符号),该图形通过外覆层是可见的。
在许多实施方案中,基底构件将为基本上平面的并且可被表征为(例如,预成形的)聚合物膜。然而,基底构件也可被构造成弯曲的、复杂的、以及三维的形状。
基底构件的厚度可以变化并且通常取决于最终制品的预期用途。在一些实施方案中,基底构件(例如膜)的厚度小于约0.5mm并且通常介于约0.02mm和约0.2mm之间。
有机聚合物基底(例如膜)构件可使用常规的成膜技术形成。可对基底构件15进行处理以改善与邻近的任何构件的粘附性。此类处理的例子包括化学处理、电晕处理(如空气或氮气电晕)、等离子体、火焰或光化辐射。层间粘附力可使用任选的施用的接合层或底漆层来改善。
当成品旨在用于显示面板时,制品10的基底构件15和其他组件(例如,粘合剂18、硬质涂层17、硅质层13和表面层14)通常也是透光的,如前文所述。
适当的透光性光学膜基底构件包括例如多层光学膜(例如美国专利6,991,695(Tait等人)和WO 99/36248(Neavin等人)、微结构化膜(例如逆向反射片材和增亮膜)(例如,反射性或吸收性)、偏振膜、漫射膜、以及延迟膜(例如,双轴延迟膜)和补偿膜,例如美国专利7,099,083(Johnson等人)中所描述的那些。
主体构件12的前表面的至少一部分以及在典型实施方案中的其整个前表面能够与硅氧烷键合,即,与疏水硅烷化合物能够形成硅氧烷键。
这种能力通过在主体构件12的表面上形成硅质层13来提供。
硅质层通常为具有低孔隙率水平的连续层。例如,当硅质层包括如WO2012/173803中所述的酸烧结纳米粒子的干燥网络时,烧结纳米粒子的硅质层具有20体积%至50体积%,25体积%至45体积%,或30体积%至40体积%的孔隙率。孔隙度可根据例如W.L.Bragg和A.B.Pippard,Acta Crystallographica(晶体学报),6,865(1953)中的公布的工序由(烧结纳米粒子)底漆层涂层的折射率计算。相比之下,本文所述的硅质层具有小于20体积%、15体积%或10体积%的孔隙率。在一些实施方案中,硅质层具有小于9%、8%、7%、6%、5%、4%、3%、2%或1%的孔隙率。
还如WO2012/173803中所述,当硅质层包括烧结纳米粒子时,孔隙率趋于与表面粗糙度相关。也就是说,表面粗糙度增大往往会导致疏水性增强。
然而,低孔隙率和减小的粗糙度可有助于改善阻隔性能,从而防止油墨或其他表面污染物渗到外疏水性硅烷层之外。硅质层与(例如,填充好的)疏水性硅烷表面层一起可在表面上提供书写笔迹的保持。当记号笔油墨渗透进表面内时,可能发生干擦笔迹的拖毛,使得难以或不可能用干擦除器通过简单的揩擦而移除。如果书写表面多孔或柔软,则往往发生这种渗透。本发明提供了不多孔的书写表面,从而防止因溶剂渗透进书写表面中而导致拖毛。
据报道,熔融二氧化硅折射率为1.458。由于空气的折射率为1.0,因此多孔硅质层具有比熔融二氧化硅更低的折射率。例如,当硅质层具有20体积%的孔隙率时,计算出的折射率将为1.164。
在一些实施方案中,硅质层13还包含碳。例如,硅质层可包含约10原子%至约50原子%的碳。由于包含碳与低孔隙率的组合,硅质层可具有大于1.458(即,熔融二氧化硅)的折射率。例如,硅质层的折射率可为至少1.48、1.49、1.50、1.51、1.52、1.53、1.54、1.55、1.56、1.57、1.58、1.59或1.60。当碳含量从30原子%的碳增加到50原子%的碳时,折射率也增加。在一些实施方案中,折射率可在至多2.2的范围内。
硅质层的原子组成(例如,硅、碳、氧)可通过化学分析电子光谱法(ElectronSpectroscopy for Chemical Analysis,ESCA)来测定。Si-C键合的存在可通过傅立叶变换红外光谱(Fourier Transform Infrared Spectroscopy,FTIR)来测定。光学特性(例如折射率)可通过椭圆偏光法(Ellipsometry)来测定。
在一个有利的实施方案中,硅质层为钻石样玻璃(“DLG”)膜,诸如美国专利6,696,157(David等人)所述。此类材料的优点在于,除了在主体构件上提供硅氧烷可键合的前表面之外,此类DLG还可提供改善的刚度、尺寸稳定性和耐久性。这在基底构件下面的组分相对较软的时候尤其有益。
适用于本发明的示例性钻石样玻璃材料包含含有碳、硅、氢和氧的富碳钻石样无定型共价体系。无定形硅质(例如DLG)层不存在结晶度可通过X射线衍射(X-RayDiffraction,XRD)来确定。通过将基底置于射频(“RF”)化学反应器中的通电电极上,在离子轰击条件下沉积包含碳、硅、氢和氧的致密无规共价体系而生成DLG。在特定的实施中,在四甲基硅烷和氧混合物的强烈离子轰击条件下沉积DLG。通常,DLG在可见光与紫外光区表现可忽略的光学吸收,即约250nm至约800nm。另外,与其它类型的含碳膜相比,DLG通常对挠曲断裂表现出改善的抗性,并对包括陶瓷、玻璃、金属和聚合物的许多基底表现出优异的粘附性。
DLG通常包含至少约30原子%的碳,至少约25原子%的硅,以及小于或等于约45原子%的氧。DLG通常包含约30原子%至约50原子%的碳。在特定的具体实施中,DLG可包含约25原子%至约35原子%的硅。另外,在某些具体实施中,DLG包含约20原子%至约40原子%的氧。在特定有利的具体实施中,在不含氢的基础上,DLG包含约30原子%至约36原子%的碳,约26原子%至约32原子%的硅,以及约35原子%至约41原子%的氧。“不计氢”指的是通过诸如化学分析电子光谱(ESCA)的方法确定的物质的原子组成,所述方法即使薄膜中存在大量的氢也不检测氢。
该(例如DLG)硅质层可制成特定厚度,通常在至少50nm、75nm或100nm至10微米的范围内。在一些实施方案中,该厚度不大于5微米、4微米、3微米、2微米或1微米。在一些实施方案中,厚度小于1微米、900nm、800nm、700nm、600nm、500nm、400nm、300nm或200nm。
在典型的实施方案中,该(例如DLG)硅质层具有足够的柔韧性,使得其通过在下文实施例中描述的弯曲测试(Bend Test)。当将该(例如DLG)硅质层施加到足够柔韧的基底如(例如PET)有机聚合物膜上时。该制品也足够柔韧,使得制品通过弯曲测试(Bend Test)。甚至还包括硬质涂层的制品也可表现出此类柔韧性。
硅质层13还包括表面层14,其包含键合到下面的(例如DLG)硅质层13上的至少一种C8-C36烃硅烷化合物硅氧烷。
硅烷化合物含有反应性甲硅烷基和疏水性烃基两者。反应性甲硅烷基团具有至少一个可与DLG层反应的羟基基团或可水解基团。疏水性烃基通常包括C8-C36烷基、芳基、或它们的组合。
在一些实施方案中,表面层包括键合到下面的硅质表面的C18-C36烃硅烷化合物硅氧烷的反应产物的至少一个单层。由DLG例示的硅质层可表征为平面化层,从而在基底上提供平滑表面。在一些实施方案中,硅质层具有小于1微米、500nm、100nm、75nm、50nm、25nm或10nm的表面粗糙度(Ra)。此类表面适用作例如剥离层。与本领域所述的压敏粘合剂的剥离层不同,所述隔离层共价连接(即,键合)到(例如DLG)硅质层上,从而提供耐用的隔离表面。
在其他实施方案中,表面层包括至少一种C8至C17烃硅烷化合物与至少一种C18-C36烃硅烷化合物的混合物的反应产物的至少一个单层,两种化合物的硅氧烷均键合到下面的硅质表面上。因此,该(例如填充好的)单层C18-C36烃因C8至C17烃的存在而遭到破坏,从而提供合适的表面张力以获得良好的油墨接受性。此类表面适用作例如可书写的干擦表面。
疏水性烃层通常为一种或多种硅烷化合物的反应产物,该硅烷化合物具有下式(I):
R1-Si(R2)3-x(R3)x
(I)
在式(I)中,基团R1独立地为C8-C36烷基、芳基、或它们的组合(例如烷基芳基或芳基烷基)。每个R2独立地为羟基或可水解的基团。每个R3独立地为不可水解的基团。每个变量x为等于0、1、或2的整数。
在一些实施方案中,合适的烷基R1基团具有至少6个、7个、或8个、并且通常不超过36个碳原子。合适的芳基R1基团通常具有6至18个碳原子、6至12个碳原子、或6至10个碳原子。一些示例性的芳基为苯基、二苯基和萘基。一些示例性的亚芳基为亚苯基、二亚苯基和亚萘基。
值得注意的是,R1不含氟取代基并且不含硅氧烷取代基,诸如二烷基(甲基)硅氧烷重复单元。
每个硅烷化合物具有至少一个式-Si(R2)3-x(R3)x的基团。每个基团R2独立地为羟基或可水解的基团。每个基团R3独立地为不可水解的基团。变量x为等于0、1、或2的整数。硅烷化合物具有单个甲硅烷基基团,并且R1是一价的。
在每个式-Si(R2)3-x(R3)x的基团中,可存在一个、两个或三个R2基团。R2基团为与下面的硅质(例如DLG)层反应的反应位点。即,可水解基团或羟基与硅质(例如DLG)层DLG层的表面反应以共价连接硅烷化合物,从而形成–Si-O-Si-键。合适的可水解R2基团包括例如烷氧基、芳氧基、芳烷基氧基、酰氧基或卤素基团。合适的烷氧基基团通常具有1至10个碳原子、1至6个碳原子、1至4个碳原子或1至3个碳原子。合适的芳氧基基团通常具有6至12个碳原子或6至10个碳原子,例如苯氧基。合适的芳烷基氧基基团通常具有含1至10个碳原子、1至6个碳原子或1至4个碳原子的烷氧基基团和含6至12个碳原子或6至10个碳原子的芳基基团。示例性的芳烷基氧基基团具有含1至4个碳原子的烷氧基基团以及共价附接到该烷氧基基团的苯基基团。合适的卤素基团可为氯、溴或碘,但通常为氯。合适的酰氧基基团具有式–O(CO)Rb,其中Rb为烷基、芳基或芳烷基。合适的烷基Rb基团常常具有1至10个碳原子、1至6个碳原子、或1至4个碳原子。合适的芳基Rb基团通常具有6至12个碳原子或6至10个碳原子,例如苯基。合适的芳烷基Rb基团通常具有含1至10个碳原子、1至6个碳原子或1至4个碳原子并且被含6至12个碳原子或6至10个碳原子的芳基例如苯基取代的烷基基团。当存在多个R2基团时,它们可为相同或不同的。在许多实施方案中,每个R2为烷氧基或氯基。
如果在每个式-C(R1)2-Si(R2)3-x(R3)x的基团中存在少于三个R2基团,则存在至少一个R3基团。R3基团为不可水解基团,其不是R1。当所有不可水解基团独立地为R1时,x=0并且不存在R3基团。许多烷基、芳基和芳烷基是不可水解的基团。合适的烷基基团包括那些具有1至5个碳原子、1至4个碳原子或1至3个碳原子的基团。当存在多个R3基团时,这些基团可以相同或不同。
合适的硅烷化合物可购自多个供应商。含有烷基的示例性硅烷化合物包括但不限于C10H21-Si(OC2H5)3、C18H37-Si(OC2H5)3、C18H37-Si(Cl)3、和C8H17-Si(Cl)3。包含芳基基团的硅烷示例包括但不限于C6H5-Si(OCH3)3、C6H5-Si(Cl)3、和C10H7-Si(OC2H5)3。
前提条件是表面层具有足够量的键合到硅质表面上的C8-C36硅烷化合物硅氧烷,用于提供期望的剥离特性或可书写性及耐久性记号笔迹可移除性,低浓度的其他硅烷化合物(例如其中R1小于8、7或6,如C1-C4烷基或根据WO2012/173803的式Ib的硅烷化合物)可任选地存在。
在典型的实施方案中,疏水性烃层包含至少一种式1的硅烷化合物的反应产物,其中R1为包含18至36个碳原子的(例如直链)烷基。在一些实施方案中,R1具有不大于30个、26个、22个或18个碳原子。当表面层主要包含根据式1的C18硅烷化合物时,表面层不是充分可书写的,表现出干擦和耐久性记号笔两者的去湿。然而,表面层表现出良好的记号笔迹可移除性(根据实施例中所述的测试方法“4”)。此外,表面层表现出低剥离粘附力,并且适用作压敏粘合带的剥离层。在一些实施方案中,当使用Magic进行测量时,用于剥离层的表面层的剥离粘附力通常小于100克/英寸、75克/英寸、50克/英寸或25克/英寸。
在一些实施方案中,表面层包含一种或多种根据式1的硅烷化合物,其中R1包含6至16个碳原子。此类表面层是可书写的,未表现出干擦和耐久性记号笔两者的去湿。然而,此类表面层不具有足够的耐久性记号笔迹可移除性(根据实施例中所述的测试方法“3”)。
在其他实施方案中,表面层包含一种或多种根据式1的硅烷化合物的组合,其中R1包含6至16个碳原子和一种或多种根据式1的硅烷化合物,其中R1包含18至36个碳原子。通过使用此类硅烷化合物的组合,可保持可书写能力,同时优化耐久性记号笔迹可移除性(根据实施例中所述的测试方法“4”)。
可使用第一C8-C17硅烷化合物和第二C18-C36硅烷化合物的各种组合。一般来讲,第一C8-C17硅烷化合物的按重量计的量大于第二C18-C36硅烷化合物的按重量计的量。在一些实施方案中,例如当第一硅烷化合物为C8时,第一硅烷化合物对第二硅烷化合物的重量比优选大于1:1,但小于19:1。在其他实施方案中,例如当第一硅烷化合物为C16时,第一硅烷化合物对第二硅烷化合物的重量比优选大于4:1,但可达到最多19:1或更大的范围。第一硅烷化合物对第二硅烷化合物的最大重量比可为40:1、35:1、30:1、或25:1。
在硅质(例如DLG)层的表面处理(即与底漆层的反应)中,硅烷化合物通常可以以纯净形式使用(例如,硅烷化合物可通过化学气相沉积而施用)。另选地,可将硅烷化合物与一种或多种有机溶剂和/或一种或多种其他任选的化合物混合,形成涂料组合物。
可用于表面层涂料组合物的合适有机溶剂包括但不限于:脂肪醇类,例如甲醇、乙醇和异丙醇;酮类,诸如例如丙酮和甲基乙基酮;酯类,例如乙酸乙酯和甲酸甲酯;醚类,例如乙醚、二异丙醚、甲基叔丁基醚和二丙二醇单甲醚(DPM);烷烃类,例如庚烷、癸烷和其他石蜡族(即,烯烃(oleofinic))溶剂;以及各种氟化溶剂。
如果使用有机溶剂,则以含溶剂涂料组合物的总重量计,涂料组合物通常含有可溶解或悬浮至少约0.01重量%、0.1重量%、或1重量%的硅烷化合物的有机溶剂量。在一些实施方案中,硅烷化合物的量按涂料组合物的重量计在至多3重量%、4重量%或5重量%的范围内。
值得注意的是,可书写表面层的耐久性记号笔迹可移除性由式1的化合物提供。因此,不需要包括其他低表面能材料,例如氟烃或硅氧烷单体、低聚物或聚合物。因此,可书写表面层和硬质涂层组合物可不含此类组分。
表面层可任选地包含少量其他材料。当存在时,此类材料占烃硅氧烷键合表面层的不大于10重量%、9重量%、8重量%、7重量%、6重量%、5重量%、4重量%、3重量%、2重量%、1重量%、0.5重量%、0.1重量%、0.005重量%、0.001重量%。因此,如前所述,表面层包含至少90重量%、91重量%、92重量%、93重量%、94重量%、95重量%、96重量%、97重量%、98重量%、99重量%或更多的根据式1的硅烷化合物的反应产物。
在一些实施方案中,诸如图2所示,在硅质(例如DLG膜)层和有机聚合物(例如膜)主体构件之间提供硬质涂层。
硬质涂层可改善硅质层和有机聚合物主体构件15之间的粘附性。硬质涂层还可改善刚度、尺寸稳定性和耐久性;尤其是当硅质层具有最小厚度时。
可书写表面层的硬质涂层是一种或多种可聚合单体、低聚物和/或聚合物的反应产物。在一些实施方案中,硬质涂层还包含颗粒或纳米粒子。
可聚合材料可以是例如可自由基聚合的、可阳离子聚合的和/或可缩聚的。可用的可聚合材料包括例如丙烯酸酯和甲基丙烯酸酯、环氧化物、多异氰酸酯和三烷氧基硅烷封端的低聚物和聚合物。优选地,所述可聚合材料包含可自由基聚合的材料。
优选地,可聚合材料包含可自由基聚合的材料,例如一种或多种多(甲基)丙烯酸酯单体和低聚物。
可用的多(甲基)丙烯酸酯单体和低聚物包括:
(a)包含二(甲基)丙烯酰基的单体,诸如1,3-丁二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,6-己二醇二丙烯酸酯、1,6-己二醇单丙烯酸酯单甲基丙烯酸酯、乙二醇二丙烯酸酯、烷氧化脂族二丙烯酸酯、烷氧化环己烷二甲醇二丙烯酸酯、烷氧化己二醇二丙烯酸酯、烷氧化新戊二醇二丙烯酸酯、己内酯改性的新戊二醇羟基特戊酸酯二丙烯酸酯、己内酯改性的新戊二醇羟基特戊酸酯二丙烯酸酯、环己烷二甲醇二丙烯酸酯、二乙二醇二丙烯酸酯、二丙二醇二丙烯酸酯、乙氧基化双酚A二丙烯酸酯、羟基新戊醛改性的三羟甲基丙烷二丙烯酸酯、新戊二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、二丙烯酸四乙二醇酯、三环癸二甲醇二丙烯酸酯、三乙二醇二丙烯酸酯、三丙二醇二丙烯酸酯;
(b)包含三(甲基)丙烯酰基的单体,诸如甘油三丙烯酸酯、三羟甲基丙烷三丙烯酸酯、乙氧基化三丙烯酸酯(例如,乙氧基化三羟甲基丙烷三丙烯酸酯)、丙氧基化三丙烯酸酯(例如,丙氧基化甘油三丙烯酸酯、丙氧基化三羟甲基丙烷三丙烯酸酯)、三羟甲基丙烷三丙烯酸酯、三(2-羟乙基)异氰脲酸酯三丙烯酸酯;
(c)包含更高官能度(甲基)丙烯酰基的单体,诸如双三羟甲基丙烷四丙烯酸酯、二季戊四醇五丙烯酸酯、季戊四醇三丙烯酸酯、乙氧基化季戊四醇四丙烯酸酯和己内酯改性的二季戊四醇六丙烯酸酯。
也可采用低聚(甲基)丙烯酰基单体,诸如例如聚氨酯丙烯酸酯、聚酯丙烯酸酯和环氧丙烯酸酯。
此类(甲基)丙烯酸酯单体可从供应商处广泛获得,诸如例如,宾夕法尼亚州埃克斯顿的沙多玛公司(Sartomer Company of Exton,Pennsylvania);新泽西州森林公园的氰特工业公司(Cytec Industries of Woodland Park,NJ);和威斯康辛州密尔沃基的奥德里奇化学公司(Aldrich Chemical Company of Milwaukee,Wisconsi)。
在一些实施方案中,硬质涂层组合物(例如,仅仅)包含具有至少三个(甲基)丙烯酸酯官能团的交联剂。在一些实施方案中,交联单体包含至少四个、五个或六个(甲基)丙烯酸酯官能团。丙烯酸酯官能团往往比(甲基)丙烯酸酯官能团更有利。
优选的可商购获得的交联剂包括,例如,三羟甲基丙烷三丙烯酸酯(可以商品名“SR351”从宾夕法尼亚州埃克斯顿沙多玛公司商购获得)、乙氧基化三羟甲基丙烷三丙烯酸酯(可以商品名“SR454”从宾夕法尼亚州埃克斯顿沙多玛公司商购获得)、季戊四醇四丙烯酸酯、季戊四醇三丙烯酸酯(可以商品名“SR444”从沙多玛公司商购获得)、双季戊四醇五丙烯酸酯(可以商品名“SR399”从沙多玛公司商购获得)、乙氧基化季戊四醇四丙烯酸酯、乙氧基化季戊四醇三丙烯酸酯(可以商品名“SR494”从沙多玛公司购得)、双季戊四醇六丙烯酸酯和三(2-羟乙基)异氰脲酸酯三丙烯酸酯(可以商品名“SR368”从沙多玛公司购得)。
这些单体和低聚物中的许多可表征具有高Tg,这意味着此类单体或低聚物的均聚物通常具有至少40℃、50℃、60℃、70℃、80℃、90℃或100℃的玻璃化转变温度。
在一些实施方案中,硬质涂层可包含至少5重量%、10重量%、15重量%或20重量%、典型地达到最多30重量%范围的低Tg单体或低聚物,这意味着此类单体或低聚物的均聚物一般具有小于25℃或0℃的玻璃化转变温度。各种低Tg单体和低聚物是已知的。一个代表性示例为乙氧基化三羟甲基丙烷三丙烯酸酯(Tg=-40℃)
硬质涂层组合物通常包含足够量的高Tg可聚合材料和纳米粒子或其他颗粒,使得可书写表面,或换句话讲包括包含C18-C36烃基的化合物的固化硬质涂层组合物是非粘性的,并且具有远高于室温的玻璃化转变温度(Tg)。在典型的实施方案中,硬质涂层的Tg为至少40℃、50℃、60 70℃、80℃、90或100℃。
在一些实施方案中,硬质涂层包含至少60重量%、65重量%、70重量%、75重量%或80重量%的烯键式不饱和单体或具有至少两个烯键式不饱和基团的低聚物的聚合单元。在一些实施方案中,硬质涂层包含至少60重量%、65重量%、70重量%、75重量%或80重量%的烯键式不饱和单体或具有至少三个、至少四个或至少五个烯键式不饱和基团的低聚物的聚合单元。
取决于可聚合材料的选择,前体组合物可任选地含一种或多种有助于聚合所述可聚合材料的固化剂。对于特定的可聚合材料,固化剂的选择取决于可共聚材料的化学性质。例如,就环氧树脂而言,通常选择已知用于环氧树脂的固化剂(例如双氰胺、鎓盐或聚硫醇)。就可自由基聚合的树脂而言,自由基热引发剂和/或光引发剂是可用的固化剂。
通常,任选的固化剂以有效促进单体聚合的量使用,所述量将随例如固化剂的类型、固化剂的分子量和聚合方法而异。任选的固化剂通常以占前体组合物总重量的约0.01重量%至约10重量%的量包含在前体组合物中,但也可使用更高和更低的量。硬质涂层前体组合物可例如通过暴露于热源(例如热、红外辐射)、电磁辐射(例如紫外和/或可见辐射)和/或颗粒辐射(例如γ辐射的电子束)而固化。
可用的自由基光引发剂包括例如安息香醚(如安息香甲基醚和安息香异丙基醚)、取代的安息香醚(例如茴香偶姻甲基醚)、取代的苯乙酮(例如2,2-二甲氧基-2-苯基苯乙酮)、取代的α-酮醇(例如2-甲基-2-羟基苯丙酮)、二苯甲酮衍生物(例如二苯甲酮)、以及酰基膦氧化物。示例性的市售光引发剂包括以商品名“IRGACURE”(例如IRGACURETM651、IRGACURETM184和IRGACURETM819)或“DAROCUR”(例如DAROCURTM1173、DAROCURTM4265)来自纽约州Tarrytown的汽巴公司(Ciba Specialty Chemicals,Tarrytown,New York)和以商品名“LUCIRIN”(例如“LUCIRIN TPO”)来自新泽西州帕西帕尼的巴斯夫(BASF,Parsippany,New Jersey)的那些。
在典型实施方案中,硬质涂层包含纳米粒子。对于给定的材料,纳米粒子可在已知的粒度分布上具有一系列粒度。在一些实施方案中,平均粒度可在约1nm至约100nm范围内。粒度和粒度分布可以已知的方式确定,包括例如通过透射电子显微镜(“TEM”)确定。合适的纳米粒子可包括多种材料中的任何材料,例如选自氧化铝、氧化锡、氧化锑、二氧化硅、氧化锆、二氧化钛的金属氧化物及前述两者或更多者的组合。经表面改性的胶态纳米粒子可基本上完全凝结。
在一些实施方案中,二氧化硅纳米粒子的粒度可为约5nm至约75nm。在一些实施方案中,二氧化硅纳米粒子的粒度可为约10nm至约30nm。二氧化硅纳米粒子可以约10重量%至约95重量%的量存在于固化硬质涂层组合物中。在一些实施方案中,二氧化硅纳米粒子以至少25重量%、30重量%,35重量%,40重量%,45重量%或50重量%的量存在,并且通常不大于70重量%的固化硬质涂层。
适用的二氧化硅纳米粒子可以商品名NALCO.TM从伊利诺伊州纳波维尔的纳尔科化学公司(Nalco Chemical Co.(Naperville,Ill.))商购获得。胶态二氧化硅。合适的二氧化硅产品包括NALCOTM。产品1040、1042、1050、1060、2327和2329。合适的热解法二氧化硅产品包括例如以商品名AEROSILTM系列OX-50、-130、-150、和-200由德国哈瑙的德固萨公司(DeGussa AG(Hanau,Germany))销售的产品,以及CAB-O-SPERSE.TM.2095、CAB-O-SPERSE.TM.A105、CAB-O-SIL.TM.MS,它们得自伊利诺伊州塔斯科拉的卡博特公司(CabotCorp.(Tuscola,Ill.))。
纳米粒子可以是经表面改性的,这指纳米粒子具有经改性的表面以使得纳米粒子提供稳定分散体的事实。“稳定分散体”指这样的分散体:在分散体中,胶态纳米粒子在环境条件下例如在室温(约20℃至约22℃)、大气压力并无极端电磁力下静置一段时间例如约24小时后不团聚。表面处理使纳米粒子稳定,以使得这些微粒将很好地分散在可涂覆型组合物中并得到基本上均质的组合物。此外,可在纳米粒子表面的至少一部分上用表面处理剂进行改性,以使得经稳定化的颗粒在固化过程中可与可涂布组合物共聚或反应。
金属氧化物纳米颗粒可以用表面处理剂处理,以使它们适用于本发明。一般来讲,表面处理剂具有第一末端和第二末端,所述第一末端将附接至颗粒表面(通过共价键、离子键或强物理吸附作用),所述第二末端使颗粒与可涂覆型组合物相容,和/或在固化过程中与可涂覆型组合物反应。表面处理剂的示例包括醇、胺、羧酸、磺酸、膦酸、硅烷和钛酸盐。处理剂的类型可取决于金属氧化物表面的性质。例如,对于二氧化硅和其它含硅填料,硅烷通常是优选的。表面改性可紧随与可涂覆组合物混合完成,或在混合后完成。就硅烷而言,优选在颗粒或纳米颗粒被掺入可涂覆组合物之前使硅烷与颗粒或与纳米颗粒的表面发生反应。表面改性剂的量取决于若干因素,例如粒度、颗粒类型、改性剂分子量、和改性剂类型。一般来讲,单层的改性剂附接至颗粒表面。所需的附接过程或反应条件也取决于所用的表面改性剂。对于硅烷,表面处理可在酸或碱的条件下在高温下进行约1小时到至多约24小时的时间。
表面处理剂是本领域已知的,包括例如异辛基三甲氧基硅烷、N-(3-三乙氧基甲硅烷基丙基)氨基甲酸甲氧基乙氧基乙氧基乙酯(PEG3TES)、SILQUEST.TM.A1230、N-(3-三乙氧基硅烷基丙基)氨基甲酸甲氧基乙氧基乙氧基乙酯(PEG2TES)、3-(甲基丙烯酰氧基)丙基三甲氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、3-(甲基丙烯酰基氧基)丙基三乙氧基硅烷、3-(甲基丙烯酰氧基)丙基甲基二甲氧基硅烷、3-(丙烯酰基氧基丙基)甲基二甲氧基硅烷、3-(甲基丙烯酰基氧基)丙基二甲基乙氧基硅烷、3-(甲基丙烯酰基氧基)丙基二甲基乙氧基硅烷、乙烯基二甲基乙氧基硅烷、苯基三甲氧基硅烷、正辛基三甲氧基硅烷、十二烷基三甲氧基硅烷、十八烷基三甲氧基硅烷、丙基三甲氧基硅烷、己基三甲氧基硅烷、乙烯基甲基二乙酰氧基硅烷、乙烯基甲基二乙氧基硅烷、乙烯基三乙酰氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三异丙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三苯氧基硅烷、乙烯基三-叔丁氧基硅烷、乙烯基三-异丁氧基硅烷、乙烯基三异丙烯氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、苯乙烯基乙基三甲氧基硅烷、巯基丙基三甲氧基硅烷、3-缩水甘油氧基丙基三甲氧基硅烷、丙烯酸、甲基丙烯酸、油酸、硬脂酸、十二烷酸、2-[2-(2-甲氧基乙氧基)乙氧基]乙酸(MEEAA)、丙烯酸β-羧基乙基酯、2-(2-甲氧基乙氧基)乙酸、甲氧基苯基乙酸、以及上述两种或更多种物质的混合物。
胶态分散体中的颗粒的表面改性可以多种方式实现。所述方法涉及无机分散体与表面改性剂以及任选地共溶剂的混合物,所述共溶剂例如1-甲氧基-2-丙醇、乙醇、异丙醇、乙二醇、N,N-二甲基乙酰胺和1-甲基-2-吡咯烷酮。添加所述共溶剂能够提高表面改性剂及经表面改性的颗粒的溶解度。包含无机溶胶和表面改性剂的混合物随后在室温或升高的温度下在混合或不混合的情况下反应。在一种方法中,混合物可在约85℃下反应约24小时,得到表面改性的溶胶。在对金属氧化物进行表面改性的一种方法中,金属氧化物的表面处理可涉及将酸性分子吸附到颗粒表面。重金属氧化物的表面改性优选在室温下进行。
在一些实施方案中,至少一部分纳米粒子可以以上述方式进行表面改性。在其他实施方案中,所有纳米粒子均经表面改性。在其他实施方案中,所有纳米粒子均不经表面改性。
可聚合硬质涂层组合物可以通过如下方式形成:将可自由基聚合的材料溶解于相容性有机溶剂中,然后与固体浓度为约60%至70%的纳米粒子分散体组合。可采用前述有机溶剂中的一种或它们的共混物。
可使用常规膜涂覆技术将硬质涂层组合物以单层或多层涂覆到(例如,显示器表面或膜)基底。可使用多种技术进行薄膜涂覆,包括浸渍涂布、正向和反向辊涂布、线绕棒涂布和模具涂布。模具涂布机包括:刮刀涂布机、槽式涂布机、滑动式涂布机、液压轴承涂布机、滑动幕式涂布机、降模幕式涂布机和挤出涂布机等等。文献中描述了多种类型的模具涂布机。尽管基底通常可以方便地为成卷的连续料片的形式,但涂层可以涂覆到单独的片材上。
将硬质涂层组合物在烘箱中进行干燥以除去溶剂,然后优选地在惰性气氛下(氧含量低于50ppm)例如通过暴露于在所需波长下的紫外辐射(使用H灯泡或其它灯)来进行固化。该反应机制引起可自由基聚合的材料交联。
固化的硬质涂层表面层的厚度通常为至少0.5微米、1微米或2微米。硬质涂层的厚度一般不大于50微米或25微米。优选地,厚度在约5微米到15微米的范围内。
在一个实施方案中,用于制备实施方案的制品的方法包括:(a)提供具有(例如前)表面的有机聚合物(例如膜)基底构件,其中该表面的至少一部分包括硅质(例如DLG)薄膜层;(b)将前述C8-C36硅烷化合物施加到硅质层的至少一部分上;以及(c)(例如,热)固化,使得硅烷化合物的甲硅烷基基团与硅质(例如DLG)薄膜层形成硅氧烷键。
在另一个实施方案中,用于制备实施方案的制品的方法包括:(a)提供有机聚合物(例如膜)基底构件层,其具有(例如前)表面,(b)通过(b1)施加硬质涂层组合物和(b2)固化该硬质涂层组合物在前表面上提供硬质涂层;(c)将硅质(例如DLG)薄膜层沉积在硬质涂层组合物上;(d)提供表面层,这通过(d1)将前述C8-C36硅烷化合物施加到硅质层的至少一部分上;和(d2)(例如,热)固化,使得硅烷化合物的甲硅烷基基团与硅质(例如DLG)薄膜层形成硅氧烷键来进行。
与表征为“亲水性的”US2014/0329012的表面层不同,本文所述的表面层是疏水性的。术语“疏水性的”是指水滴或水性溶液液滴在其上显示具有至少50度、至少60度、至少70度、至少80度、或至少85度静态水接触角的表面。在一些实施方案中,静态水接触角小于100度、95度或90度。
在一些实施方案中,表面层易于清洁,这通过干擦和耐久性记号笔迹可移除性得到证实。期望易于清洁的示例性应用包括窗口、电子设备屏幕、工作表面、器具、门和墙壁表面、标牌等。在这个实施方案中,表面层可以为不可书写的。
在一些实施方案中,制品为干擦制品或其组件。干擦制品可进一步包括其他任选组件,诸如框架、用于储存材料及工具(诸如书写器具、擦除器、布、信纸等)的装置、用于载运的手柄、保护盖、用于悬挂于垂直表面上的装置、画架等。
期望包括可书写表面的文件夹、笔记本、活页夹等的其他制品,其中将有效的可书写性与随后易于移除书写痕迹相结合。
可书写表面层通常不表现出干擦记号笔和耐久性记号笔两者的去湿。
如WO 2011/094342所述,干擦记号笔中的溶剂组合物通常列于记号笔上或者记录于用于记号笔的MSDS上。用于干擦记号笔的通用溶剂包括(例如)乙醇、异丙醇、甲基异丁基酮、和乙酸正丁酯。具有高表面张力的一种溶剂为乙酸正丁酯,其具有约25mJ/m2的表面张力。因此,在一些实施方案中,可通过表面张力为约25mJ/m2或更低的溶剂来润湿干擦表面。在一个实施方案中,书写表面的表面能在约26mJ/m2至低于约38mJ/m2的范围内。在一个实施方案中,书写表面的表面能在约30mJ/m2至低于约38mJ/m2的范围内。
耐久性记号笔可具有与干擦记号笔相同的许多溶剂。然而,由于耐久性记号笔的其他组分,耐久性记号笔在溶剂蒸发后通常是“防水的”,并且是不可干擦的。例如,如果在一片玻璃上绘制1英寸的实心正方形并使其干燥24小时,则通常可使用下文实施例中描述的干擦记号笔书写可擦除性测试来除去来自干擦记号笔的油墨。然而,用耐久性记号笔(例如黑色SharpieTM)在一片玻璃上绘制1英寸的实心正方形并使其干燥24小时,不能使用该相同测试来移除。
与描述通过简单地加水(例如,室温下的自来水)和/或水蒸气(例如,人哈气)并擦拭以从表面去除耐久性记号笔迹的US2014/0329012相比,可根据实施例中所述的测试方法用干纸巾去除耐久性记号笔的笔迹。
可使用多种其他干擦类型。擦除器材料的示意性实例包括合成和/或天然(例如羊毛)材料的压制和织造毡,已使用纤维素、泡沫橡胶、氯丁橡胶、布、起绒织物、三聚氰胺纤维和类似材料。优选地,所选擦除器材料不是磨蚀性的,以便提高书写表面的耐久性。
实施例
通过下列实施例进一步示出了本公开的优点和实施方案,但这些实施例中所表述的具体材料及其量以及其它条件和细节不应当被解释为对本发明的不当限制。除非另外指明,否则在这些实施例中,所有百分比、比例和比率均按重量计。
除非另外指明或显而易见,否则所有材料都可从例如威斯康星州密尔沃基的西格玛-阿尔德里奇化学公司(Sigma-Aldrich Chemical Company;Milwaukee,WI)商购获得,或是本领域技术人员已知的。
这些缩写用于以下实施例中:g=克,hr=小时,kg=千克,min=分钟,mol=摩尔;cm=厘米,mm=毫米,mL=毫升,L=升,MPa=兆帕斯卡,并且wt=重量。
材料
测试方法
干擦/耐久性记号笔迹去湿测试
将14种不同的记号笔(选自上面列出的总共7个品牌的干擦和耐久性记号笔)用于该测试。从每个品牌选择两种颜色的记号笔,一个为黑色,另一个选自红色、绿色或蓝色。测试根据如下所述制备的实施例和比较例制备的样品。测试样品的尺寸为约6英寸乘11英寸(15.0cm乘27.9cm)。为每个记号笔品牌保留约2.5cm宽的样品水平带(即,沿着样品的宽度)。用第一记号笔在该2.5cm宽带的左手侧上写下记号笔品牌名,并用第二记号笔在该2.5cm宽带的右手侧上写下同一记号笔品牌名。这样,每个记号笔品牌书写的所有笔迹(即,品牌名)排列成一条可擦除的水平线。在用测试样品上所有品牌的每个记号笔标记之后,目视检查每条油墨线(对每个品牌)的去湿。干擦油墨的去湿(即,成珠)由油墨线中目视出现间隙或油墨线的收缩而得到证实。
干擦记号笔书写可擦除性测试
将根据下述实施例和比较例制备的样品的表面用14种干擦记号笔标记,然后置于烘箱中以允许标记在50℃下干燥一周。然后将膜样品从烘箱中取出并冷却至室温,随后置于坚硬的平坦表面上。使用EXPO橡皮擦(以商品名“EXPO DRY-ERASE ERASERS”得自伊利诺伊州贝尔伍德的桑福德公司(Sanford Corporation,Bellwood,Illinois))擦除该书写笔迹。与书写表面接触的橡皮擦面积为约12.5cm×5cm。将称重为2.5kg的12.5cm×5cm黄铜置于橡皮擦的顶部,产生0.4N/cm2的压力。在无附加手动压力的情况下,进行来回运动使承重橡皮擦通过第一标记线,直到完成十次来回运动(总共通过标记10次)。然后根据以下标准,对样品进行视觉评估并评定其可擦除性。1:>75%的油墨保留在表面上;2:50-75%的油墨保留在表面上;3:25-50%的油墨保留在表面上;4:<25%的油墨保留在表面上。
耐久性记号笔书写可擦除性测试
通过用纸巾摩擦样品的标记表面来评估根据下述实施例和比较例利用耐久性记号笔标记而制备的样品表面的可擦除性。利用适度的压力(2.9磅/1平方英寸的接触表面的擦拭介质),用手擦拭标记的膜,进行来回运动(每秒3次来回),直到标记被完全擦除,或者直到完成十次来回运动(在标记上总共来回10次)。然后根据以下标准,对膜样品进行视觉评估并评定其可擦除性。1=用纸巾擦拭对标记无影响;2=标记被部分移除并且仍然可辨认;3=大部分标记被移除,带有明显的油墨拖尾;4=标记被完全且干净地移除。
剥离力测量测试
在滑移/剥离测试仪(IMASS-2000滑移/剥离测试仪,得自马萨诸塞州阿科德的艾玛氏公司IMASS(IMASS,Inc.,Accord MA))上测量用于从根据下述实施例和比较例制备的样品表面移除3M MAGIC TAPE的剥离粘附力。将10英寸(25cm)长的3M MAGIC TAPE带置于样品表面上,并且用2.04kg橡胶辊按压。以90英寸/分钟(2.29米/分钟)的速率、180度角剥离条带。记录3次平行测试的平均剥离力。
弯曲测试
根据ASTM D3111-10“用马德尔弯曲试验法测定热融胶挠性的标准试验方法(Standard Test Method for Flexibility Determination of Hot-Melt Adhesives byMandrel bend Test Method)”进行弯曲测试。将根据下述实施例制备的测试样本切成约20mm乘25mm的片材。然后将每个片材在1秒内围绕具有6.4mm(1/4英寸)直径的金属棒缠绕180度,样本的涂覆侧位于芯轴的外侧。然后将样本从芯轴上移除并目视检查。“通过(PASS)”等级意指涂层或基底不存在可见的断裂、龟裂或开裂,或者涂层与基底发生脱粘。另选地,“不通过(FAIL)”等级意指涂层或基底出现可见的断裂、龟裂或开裂,或者涂层与基底发生脱粘。
静态水接触角测试
对根据下文所述的实施例和比较例制备的干燥样品进行水接触角测量。去离子水,得自马萨诸塞州比尔里卡的密理博公司(Millipore Corporation(Billerica,MA))。所用的接触角分析仪是来自瑞典黑格斯滕的FIBRO System AB公司(FIBRO System AB,Hagersten,Sweden)的PGX+视频接触角分析仪。使用内置照相机对由一体化泵递送的水滴(0.5μL)测量接触角。所记录的值是至少4次单独测量的平均值。
表面改性的二氧化硅纳米粒子的制备
向12升烧瓶中装入3000g含水胶态二氧化硅溶液NALCO2327,并且开始搅拌。然后加入3591g 1-甲氧基-2-丙醇。在单独的容器中混合189.1g3-甲基丙烯酰氧基丙基三甲氧基硅烷(A-174)与455g 1-甲氧基-2-丙醇。将该预混溶液加入烧瓶中,用455g 1-甲氧基-2-丙醇冲洗。将混合物在80℃下加热约16小时。将混合物冷却至35℃。用收集瓶对混合物进行真空蒸馏(30托-35托(4kPa-6.67kPa),35℃至40℃)。在蒸馏过程中,将另外的1813.5g 1-甲氧基-2-丙醇加入反应烧瓶。共收集6784g馏出液。通过在105℃烘箱中在配衡铝锅中将少量样品干燥60分钟来测定混合物的固体%。测得混合物包含52.8%的固体。加入另外的250g 1-甲氧基-2-丙醇,并搅拌混合物。测定固体%,结果为48.2%。通过用干酪包布过滤收集混合物,以移除粒子碎片。
一般涂覆过程
将约6英寸(15cm)宽的PET膜幅材用作基底。使用凹版涂布方法将含有SR 444、A174、表面改性的二氧化硅纳米粒子和ESACURE ONE(以43:5:50:2的重量比)的硬质涂层溶液涂布到PET基底上。将经硬质涂布的样品在60℃下干燥30秒,然后以20英寸/分钟(6.1米/分钟)的速率暴露于紫外光(得自马里兰州盖瑟斯堡美国贺利氏特种光源有限公司(HareusNoblelight America,LLC,Gaithersburg,MD)的300W H-灯泡)。紫外灯位于样品上方约1英寸(2.5cm)处,并且在固化期间用氮气吹扫干燥硬质涂层的表面。用于紫外固化的能量输入为60毫焦耳UVC辐射。膜上硬质涂层的干燥厚度为4微米-5微米。以此方式施加的硬质涂层在下文中称为“标准硬质涂层”。
使用2-步幅材工艺,将DLG层沉积到如上所述制备的硬质涂布的PET膜的固化硬质涂层表面上。使用在美国专利5,888,594(David等人)中详述的房屋建造等离子处理系统,进行一些修改:将转筒电极的宽度增加至42.5英寸(108cm),并移除等离子体系统内两个隔室之间的隔板,使得使用涡轮分子泵进行所有泵送,并且因此在约10毫托-50毫托(1.33Pa-6.7Pa)的工艺压力下操作。
将来自上文的硬质涂布的聚合物膜卷安装在室内,将膜围绕鼓电极卷绕,并固定到鼓的相对侧上的收卷辊。将退绕和收卷张力分别保持在8磅(13.3N)和14磅(23.3N)下。关闭室门并将腔室抽至5×10-4托(6.7Pa)的基准压力。对于沉淀步骤,分别在200标准立方厘米/分钟和1000标准立方厘米/分钟的流动速率下引入六甲基二硅氧烷(HMDSO)和氧气,并且运行压力标称处于35毫托(4.67Pa)。通过向鼓施加射频功率使等离子体在9500瓦特的功率下启动并且鼓开始旋转,使得膜以10英尺/分钟(3米/分钟)的速度传输。继续运行,直到完成辊上的膜的全部长度。
在DLG沉积步骤完成后,禁用rf功率,停止HMDSO蒸气的流动,并且氧气流速增加到2000标准cm3/min。在流速和压力稳定时,在4000瓦下重新启动等离子体,并且幅材以10英寸/分钟(3米/分钟)的速度在相反方向上传送,压力稳定在标称14毫托(1.87Pa)。该第二等离子体处理步骤是从DLG膜上去除甲基,并且用含氧官能团如Si-OH基团取代它们,这有利于将硅烷化合物接枝到DLG膜。
在以上述方式处理整个膜卷后,禁用rf功率,停止氧气流,将室排空至大气,并且从等离子体系统中取出辊以用于进一步处理。
所得DLG层的厚度为约100nm。
最后,使用#5 Mayer棒,将硅烷涂层由硅烷溶液施加到DLG层上。硅烷溶液包含IPA中所需的硅烷(如下文实施例和比较例所述)的混合物。硅烷的浓度为相对于溶液的总重量在IPA中2重量%的硅烷。此外,硅烷混合物包含2重量%的乙酸(相对于硅烷的重量)作为催化剂。然后将硅烷涂层在280℉(137.8℃)下热固化5分钟。
实施例1-16和比较例A-F
实施例1B和实施例2-16通过使用上述“一般涂布工序”来制备。硅烷涂布溶液中C8-C18硅烷的量和重量比如下表1所汇总的变化。
实施例1A通过使用上述“一般涂布工序”来制备,不同的是在沉积DLG层之前未将硬质涂层施加到至PET膜基底上。
比较例A的样品为以原样使用而无进一步处理的裸PET膜。
比较例B为可商购获得的干擦板的表面,其以原样使用而无进一步处理。此类表面包含固化硬质涂层,该硬质涂层包含氟化丙烯酸酯添加剂。
比较例C通过使用上述“一般涂布工序”来制备,不同的是在沉积DLG层之后不施加硅烷涂层。
比较例D和比较例E通过使用上述“一般涂布工序”来制备。在硅烷涂布溶液中的硅烷为用于比较例D的PEO硅烷和用于比较例E的AQUAPHOBE CM。
使用上述测试方法测试实施例样品和比较例样品。结果归纳于下表1中。
表1:
“-”是指未测试的样品。
根据上述弯曲测试来测试实施例1A和实施例1B的样品,并且两个样品均为“通过(PASS)”等级。
使用上述测试,测试实施例1A和实施例1B样品的静态水接触角。实施例1A和实施例1B的静态水接触角分别为88.7°和85.4°。
Claims (23)
1.一种制品,所述制品包括:
表面层,所述表面层包含键合到硅质层的至少一种C8-C36烃硅烷化合物硅氧烷,所述硅质层具有不大于10%的孔隙率和不大于1微米的厚度。
2.根据权利要求1所述的制品,其中所述硅质层包含10原子%至50原子%的碳。
3.根据权利要求1-2所述的制品,其中所述硅质层为钻石样玻璃层。
4.根据权利要求1-3所述的制品,其中所述硅质层的折射率大于1.458。
5.根据权利要求1-4所述的制品,所述制品还包括有机聚合物基底构件。
6.根据权利要求5所述的制品,其中所述有机聚合物基底构件为膜。
7.根据权利要求5-6所述的制品,其中所述制品还包括设置在所述有机聚合物基底构件和钻石样玻璃层之间的硬质涂层。
8.根据权利要求7所述的制品,其中所述硬质涂层包含无机氧化物颗粒。
9.根据权利要求1-8所述的制品,其中所述至少一种C8-C36烃硅烷具有下式
R1-Si(R2)3-x(R3)x
其中R1为8-36烃基;
R2为可水解基团;
R3为非R1的不可水解基团;并且
x在0至2范围内。
10.根据权利要求9所述的制品,其中R2为羟基或C1-C4烷氧基。
11.根据权利要求9-10所述的制品,其中R1为C8-C17烷基。
12.根据权利要求9-10所述的制品,其中R1为C18-C36烷基。
13.根据权利要求9-10所述的制品,其中所述表面层包含以下物质的反应产物:
i)至少一种第一烃硅烷化合物,其中R1为C8-C17烷基;以及
ii)至少一种第二烃硅烷化合物,其中R1为C18-C36烷基。
14.根据权利要求13所述的制品,其中所述第一硅烷化合物以大于所述第二硅烷化合物的量存在。
15.根据权利要求1-14所述的制品,其中所述表面层包含至少90重量%或95重量%的C8-C36烃硅烷化合物的反应产物。
16.根据权利要求1-15所述的制品,其中所述表面层为剥离层。
17.根据权利要求1-15所述的制品,其中所述制品为干擦板。
18.根据权利要求17所述的制品,其中耐久性记号笔迹可用干纸巾从所述表面层移除。
19.一种制品,所述制品包括:
表面层,所述表面层包含键合到硅质层的至少一种C8-C22烃硅烷化合物硅氧烷,所述硅质层包含30原子%至50原子%的碳和不大于1微米的厚度。
20.根据权利要求19所述的制品,其特征还在于权利要求3-18中的任一项或组合。
21.一种涂料组合物,所述涂料组合物包含:
i)至少一种具有下式的烃硅烷化合物:
R1-Si(R2)3-x(R3)x
其中R1为C8-C17烃硅烷;
R2为可水解基团;
R3为非R1的不可水解基团;并且
x在0至2范围内;以及
ii)至少一种具有下式的烃硅烷化合物:
R1-Si(R2)3-x(R3)x
其中R1为C18-C36烃硅烷;
R2为可水解基团;
R3为不可水解基团;并且
x在0至2范围内;以及
iii)任选的有机溶剂。
22.根据权利要求21所述的组合物,其中i)和ii)以大于1:1的重量比存在。
23.根据权利要求21-22所述的组合物与硅质表面的反应产物。
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