CN113165972A - 车辆用夹层玻璃 - Google Patents
车辆用夹层玻璃 Download PDFInfo
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- CN113165972A CN113165972A CN201980078028.8A CN201980078028A CN113165972A CN 113165972 A CN113165972 A CN 113165972A CN 201980078028 A CN201980078028 A CN 201980078028A CN 113165972 A CN113165972 A CN 113165972A
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- glass
- laminated glass
- resin
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- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
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Images
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Landscapes
- Engineering & Computer Science (AREA)
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Abstract
本发明公开一种夹层玻璃,其具备对置的两张玻璃板和配置于两张玻璃板之间的中间膜。中间膜具有在温度25℃、频率1×105Hz下显示出1000MPa以上的储能模量的树脂层。夹层玻璃可以为汽车用前窗玻璃。
Description
技术领域
本发明涉及一种车辆用夹层玻璃。
背景技术
以往,作为用于像汽车那样的车辆、飞机、建筑物等的玻璃,广泛使用破碎时飞溅少的夹层玻璃。夹层玻璃通常具有被夹在两张玻璃板之间的中间膜。作为夹层玻璃用中间膜,例如使用包含聚乙烯醇缩醛树脂、离聚物树脂、丙烯酸树脂等的树脂层(例如,专利文献1~5)。
以往技术文献
专利文献
专利文献1:日本特开2016-193542号公报
专利文献2:日本特开2009-298046号公报
专利文献3:日本特开2015-151540号公报
专利文献4:日本特公昭62-028105号公报
专利文献5:日本特开2000-001345号公报
发明内容
发明要解决的技术课题
要求汽车用途中所使用的前窗玻璃等玻璃部件针对行驶时的飞石等飞溅物的碰撞的耐性即耐崩裂(chipping)性优异。另一方面,为了玻璃部件的轻量化,期望玻璃板最好尽可能薄。但是,若玻璃板变薄,则趋于难以保持充分的耐崩裂性。
因此,本发明的一侧面的目的在于实现进一步改善夹层玻璃的耐崩裂性。
用于解决技术课题的手段
本发明的一侧面涉及一种车辆用夹层玻璃,其具备:对置的两张玻璃板;及中间膜,配置于这两张玻璃板之间。所述中间膜具有在温度25℃、频率1×105Hz下显示出1000MPa以上的储能模量的树脂层。
根据本发明人等的见解,在温度25℃、频率1×105Hz下的树脂层的储能模量与夹层玻璃的耐崩裂性有相关性。飞石碰撞夹层玻璃的瞬间,在夹层玻璃的外侧的玻璃板的内侧产生拉伸应力。认为该拉伸应力是夹层玻璃破碎的主要原因。根据本发明人等进行的模拟,由碰撞产生的拉伸应力在相当于频率1×105Hz附近的时间尺度(time scale)上产生。因此,认为在频率1×105Hz下的树脂层的储能模量大,有助于提高耐崩裂性。
发明效果
根据本发明的一侧面,可提供一种耐崩裂性进一步得到改善的夹层玻璃。
附图说明
图1是表示夹层玻璃的一实施方式的剖视图。
图2是通过动态粘弹性测定而得到的主曲线的例子。
图3是表示夹层玻璃的中间膜用膜材料的一实施方式的剖视图。
具体实施方式
以下,对本发明的一些实施方式进行详细说明。但是,本发明并不限定于以下实施方式。
图1是表示夹层玻璃的一实施方式的剖视图。图1所示的夹层玻璃1具备对置的两张玻璃板11、12和配置于它们之间的中间膜5。
玻璃板11、12例如可以为像浮法玻璃、风冷强化玻璃、化学强化玻璃及双层玻璃那样的无机玻璃板。玻璃板11、12中的一个或两个也可以为树脂制的透明基板。作为透明基板,例如可以举出丙烯酸树脂基板、聚碳酸酯基板、环烯烃聚合物基板、聚酯基板等透明塑料基板。
其中一个玻璃板11的厚度可以大于另一个玻璃板12的厚度。当用作车辆的玻璃部件(例如,汽车用前窗玻璃)时,夹层玻璃1通常以更厚的玻璃板11位于车辆的外侧的朝向安装于车辆。玻璃板11的厚度相对于玻璃板12的厚度之比例如可以为1.1~3.0。但是,两张玻璃板的厚度也可以相同。玻璃板11、12的厚度例如可以为0.1mm以上、0.5mm或0.8mm以上。玻璃板11的厚度可以为0.1mm以上、0.5mm或0.8mm以上且30mm以下,也可以为0.1mm以上、0.5mm或0.8mm以上且20mm以下。玻璃板12的厚度可以为0.1mm以上、0.5mm或0.8mm以上且20mm以下,也可以为0.1mm以上、0.5mm或0.8mm以上且15mm以下。
中间膜5可以具有一层以上在温度25℃、频率1×105Hz下显示出1000MPa以上的储能模量的树脂层(以下,有时称为“耐崩裂性层”。)。中间膜5可以为单层的耐崩裂性层,也可以进一步具有耐崩裂性层以外的树脂层。
从更进一步提高耐崩裂性的观点考虑,耐崩裂性层在温度25℃、频率1×105Hz下的储能模量可以为1200MPa以上且7000MPa以下或6500MPa以下,也可以为1300MPa以上且7000MPa以下或6500MPa以下,也可以为1400MPa以上且7000MPa以下或6500MPa以下。
在温度25℃、频率1×105Hz下的储能模量能够根据通过动态粘弹性测定和时间-温度换算法则(time temperature reduction law)而制作的基准温度25℃的主曲线来求出。动态粘弹性测定例如按照依据JIS K 0129:2005的方法,在温度-30~25℃、频率0.5Hz~50Hz、应变量0.05%的条件下以拉伸测定模式进行。根据粘弹性的测定结果,通过WLF法将基准温度设为25℃而制作表示储能模量与频率的关系的主曲线,根据该主曲线能够读取在频率1×105Hz下的储能模量。图2是通过动态粘弹性测定而得到的主曲线的例子。图2所示的主曲线MC1、MC2是将基准温度设为25℃而通过WLF法得到的。在频率1×105Hz下,主曲线MC1显示出1000MPa以上的储能模量,主曲线MC2显示出小于1000MPa的储能模量。
当中间膜5由多个树脂层构成时,配置于与更厚的玻璃板11相邻的位置的树脂层可以为耐崩裂性层。由此,在以玻璃板11位于车辆的外侧的朝向将夹层玻璃1安装于车辆时,可尤其有效地发挥提高针对从外部碰撞的飞溅物的耐崩裂性的效果。
从提高耐崩裂性等观点考虑,构成中间膜5的耐崩裂性层的厚度可以为0.001~10mm或0.01~1mm。
构成中间膜5的耐崩裂性层例如含有热塑性树脂。耐崩裂性层可以进一步含有增塑剂。树脂层的储能模量例如能够根据热塑性树脂的种类及增塑剂的含量来控制。若增塑剂的量相对于热塑性树脂的量之比变大,则在温度25℃、频率1×105Hz下的储能模量通常趋于下降。
构成耐崩裂性层的热塑性树脂例如可以包含选自聚乙烯醇缩丁醛树脂、丙烯酸树脂(丙烯酸聚合物)、乙烯-乙酸乙烯酯共聚物树脂、乙烯-丙烯酸共聚物树脂、聚氨酯树脂及聚乙烯醇树脂中的至少一种,耐崩裂性层可以包含聚乙烯醇缩丁醛树脂作为热塑性树脂。在该情况下,聚乙烯醇缩丁醛树脂相对于聚乙烯醇缩丁醛树脂与其他热塑性树脂的合计量的比例可以超过85质量%,也可以为90质量%以上或95质量%以上。
耐崩裂性层中的增塑剂的含量以热塑性树脂或尤其是聚乙烯醇缩丁醛树脂的量为基准,可以为0~18质量%。通过增塑剂的含量为18质量%以下,能够明显改善夹层玻璃的耐崩裂性。从相同的观点考虑,增塑剂的含量以聚乙烯醇缩丁醛树脂的量为基准,可以为17质量%以下、16质量%以下、15质量%以下、14质量%以下、13质量%以下、12质量%以下、11质量%以下、10质量%以下、9质量%以下、8质量%以下、7质量%以下、6质量%以下或5质量%以下,且可以为0质量%以上。
增塑剂能够无特别限制地从通常用作热塑性树脂的增塑剂中选择。例如,增塑剂可以包含脂肪酸酯化合物、有机磷酸酯化合物或它们的组合。
脂肪族酯化合物例如可以为聚亚烷基二醇与脂肪族单羧酸的单酯或二酯。作为聚亚烷基二醇的例子,可以举出三乙二醇、四乙二醇及三丙二醇。作为脂肪族单羧酸的例子,可以举出丁酸、异丁酸、己酸、2-乙基丁酸、庚酸、正辛酸、2-乙基己酸、正壬酸及癸酸。脂肪族酯化合物可以为碳原子数4~8的直链或支链烷基醇与脂肪族多羧酸的酯。作为脂肪族多羧酸的例子,可以举出己二酸、癸二酸及壬二酸。
增塑剂例如可以包含选自三乙二醇单(2-乙基己酸酯)、三乙二醇二(2-乙基己酸酯)、三乙二醇二-2-乙基丁酸酯及三乙二醇二(2-乙基丙酸酯)中的至少一种脂肪族酯化合物。
作为有机磷酸酯化合物的例子,可以举出磷酸三丁氧基乙酯、磷酸异癸基苯酯及磷酸三异丙酯。
耐崩裂性层根据需要可以含有其他成分。作为其他成分的例子,可以举出抗氧化剂、无机填充剂。耐崩裂性层中的聚乙烯醇缩丁醛树脂及增塑剂的合计量的比例以耐崩裂性层或用于形成该耐崩裂性层的树脂材料的量为基准,可以为80质量%以上或90质量%以上。
(夹层玻璃的制造方法)
夹层玻璃1例如能够通过包括如下工序的方法来进行制造:形成具有对置的两张玻璃板11、12和配置于这些玻璃板11、12之间的中间膜的层叠体的工序;及对层叠体进行加热及加压而形成夹层玻璃1的工序。
具有玻璃板及中间膜的层叠体例如能够通过包括如下步骤的方法得到:将中间膜5贴合于其中一个玻璃板11的步骤;及将另一个玻璃板12贴合于中间膜5的步骤。
为了形成层叠体,例如可以使用具有构成中间层的树脂层的膜材料。图3是表示夹层玻璃的中间膜用膜材料的一实施方式的剖视图。图3所示的膜材料2具备中间膜5和覆盖中间膜5的两个面的两张基材膜21及22。例如,可以从膜材料2剥离基材膜21,并将露出的中间膜5贴合于玻璃板11。其中一个基材膜21可以为具有比另一个基材膜22的表面更加易剥离性的表面的膜。也可以不设置基材膜21或基材膜22中的一个或两个。
作为基材膜21、22的例子,可以举出聚对苯二甲酸乙二酯膜、聚丙烯膜及聚乙烯膜。例如,基材膜21、22的厚度并不受特别限制,例如可以为25~200μm。
中间膜5例如能够通过如下方法来形成:对用于形成中间膜的树脂材料进行冲压成型的方法;或将包含树脂材料及溶剂的涂液涂布于基材膜等,接着,从涂膜中去除溶剂的方法。
将为了得到夹层玻璃而对由玻璃板11、中间膜5及玻璃板12组成的层叠体进行加热及加压的条件调整为使各层充分密合。例如,在0.8~10MPa的压力、60~200℃的温度、10~120分钟的加压时间的范围内设定加热及加压的条件。
夹层玻璃1作为要求耐崩裂性的车辆用夹层玻璃而尤其有用。作为车辆用夹层玻璃的例子,可以举出汽车用前窗玻璃、汽车用侧窗玻璃、汽车用天窗及汽车用后窗玻璃。
实施例
以下,举出实施例对本发明进行进一步具体的说明。但是,本发明并不限定于这些实施例。
1.中间膜用树脂层
(实施例1)
用冲压成型机将聚乙烯醇缩丁醛(PVB)树脂(Mowital B75H,KURARAY CO.,LTD.制造,缩醛单元:71~81质量%,羟基单元:18~21质量%,乙酸乙烯酯单元:1~4质量%)在150℃、30分钟的条件下进行冲压成型而形成了厚度0.4mm的中间膜用树脂层。
(实施例2)
混合了与实施例1相同的PVB树脂100质量份和三乙二醇二(2-乙基己酸酯)(3GO)10质量份。用搅拌辊将混合物充分熔融混炼而得到了作为中间膜用树脂材料的PVB树脂组合物。用冲压成型机将所得到的PVB树脂组合物在150℃、30分钟的条件下进行冲压成型而形成了厚度0.4mm的中间膜用树脂层。
(实施例3)
除了将三乙二醇二(2-乙基己酸酯)(3GO)的量变更为15质量份以外,以与实施例2相同的方式得到了厚度0.4mm的中间膜用树脂层。
(比较例1)
除了将三乙二醇二(2-乙基己酸酯)(3GO)的量变更为20质量份以外,以与实施例2相同的方式得到了厚度0.4mm的中间膜用树脂层。
(比较例2)
除了将三乙二醇二(2-乙基己酸酯)(3GO)的量变更为30质量份以外,以与实施例2相同的方式得到了厚度0.4mm的中间膜用树脂层。
(比较例3)
用冲压成型机将非交联性的乙烯-乙酸乙烯酯共聚物(EVA)(EV170,MitsuiDupont chemical Co.,Ltd.制造,乙酸乙烯酯含量:33质量%)在150℃、30分钟的条件下进行冲压成型而形成了厚度0.4mm的中间膜用树脂层。
2.中间膜用树脂层的储能模量
从各中间膜用树脂层中切出了5mm宽度×50mm长度的条状的试验片。用千分尺(Mitutoyo Corporation制造,MDE-25MX)测定了试验片的厚度。使用动态粘弹性测定机(TAinstrument公司制造,RSA-G2)在以下条件下测定了该试验片的动态粘弹性。将保持试验片的两个夹具之间的距离设定为20mm。
传感器(transducer)
·测定模式:拉伸
·轴向力(Axial Force):100.0g
·灵敏度(Sensitivity):10.0g
·比例力模式(Proportional force Mode):恒定(Constant)
·自动调整应变模式(Auto strain adjustment mode):开启(Enable)
·应变调整(Strain adjust):15.0%
·最小应变(Minimum strain):0.01%
·最大应变(Maximum strain):5.0%
·最小力量(Minimum force):5.0%
·最大力量(Maximum force):300g
测定条件
·测试参数,起始温度(Test Parameters,Start temperature):-30℃
·保温时间(Soak time):30秒
·结束温度(End temperature):25℃
·温度步阶(Temperature step):1℃
·应变(Strain):0.05%
·对数扫描模式(Logarithmic sweep mode)
·角频率(Angular frequency):0.5Hz到50.0Hz
·每10倍频率的采样点数(Points per decade):3
根据测定结果,通过WLF法制作出将基准温度设为25℃的主曲线。根据所得到的主曲线求出了在温度25℃、频率1×105Hz下的储能模量。为了制作主曲线,利用了Trios(V3.3.1.4246)中的“TTS Wizard”的数据分析。数据分析条件如下。
TTS选项(TTS Options)
·自动位移y变量(Auto-shift y variable):全部y变量(All yvariable)
·Y位移基础(Y shit base):仅温度(Temperature only)
·自动位移类型(Auto-shit type):仅X(X only)
·移除在末端对话的位移区域(Remove shift zone on end session):否(No)
TTS设定参考曲线(TTS Set Reference Curve)
·温度曲线(Curve Temperature):25.0℃
TTS生成主曲线(TTS Generate Master Curve)
·在参考温度下生成(Generate at Reference temperature)
·模式(Model):WLF
3.夹层玻璃的制作
将各中间膜用树脂层裁剪为长度150mm、宽度67mm的大小,并将其以4个边重叠的方式贴合于长度150mm、宽度67mm、厚度1.6mm的浮法玻璃上,用棍子对整体进行了加压。将长度150mm、宽度67mm、厚度1.1mm的浮法玻璃以4个边重叠的方式贴附于露出的树脂层上,用棍子对整体进行了加压。由此,得到了浮法玻璃/中间膜/浮法玻璃的层叠体。使用设定为125℃的真空层合机将所得到的层叠体加热了25分钟。接着,在设定为150℃的高压釜中,在压力115N/cm2MPa、120分钟的条件下对层叠体进行加热及加压而得到了具有浮法玻璃(1.6mm)/玻璃中间膜/浮法玻璃(1.1mm)的结构的夹层玻璃。通过相同的操作,使用实施例或比较例的各中间膜树脂层分别制作出10张夹层玻璃。
4.夹层玻璃的耐崩裂性
将宽度约5mm、长度约67mm的压敏胶黏剂带贴附于夹层玻璃的厚度1.1mm的浮法玻璃的沿长边的两端部。将厚度6mm、宽度10.0mm的合成橡胶板(CR90度)贴合于压敏胶黏剂带上。用瞬间黏合剂将厚度3mm、长度150mm、宽度67mm的一张铁板黏合于被贴合在浮法玻璃的两端部的两个合成橡胶板上。由此,得到了夹层玻璃的端部经由合成橡胶板固定于铁板的耐崩裂性评价用的试验体。
使从飞石试验机(Suga Test Instruments Co.,Ltd.制造,JA400)的喷出管连续喷射的碎石随机地碰撞试验体的夹层玻璃的厚度1.6mm的浮法玻璃侧的面。试验条件如下。
·碰撞管前端与试验体的距离:350mm
·石头种类:玄武岩
·碎石的喷射速度:70km/h
·碎石量:每一张夹层玻璃中为240个(平均重量:0.25±0.005g)
·碰撞入射角度:相对于夹层玻璃的面的垂线为0度
·试验体温度:23±1℃
试验后,目视观察夹层玻璃,将观察到长度0.5mm以上的线状裂纹的碰撞痕迹的数量记录为起点个数。根据该结果,通过下述式计算出龟裂概率。在此,碎石数为240。
龟裂概率(%)=(起点个数/碎石数)×100
利用相同的方法对5个试验体测定龟裂概率,并求出了测定值的平均值。利用龟裂概率的平均值,以下述判定标准评价了夹层玻璃的耐崩裂性。在夹层玻璃的耐崩裂性中,“A”为最优异,“D”为最差。
A:小于1.0%
B:1.0%以上且小于1.25%
C:1.25%以上且小于3.0%
D:3.0%以上
[表1]
在表1中示出评价结果。与比较例1~3的夹层玻璃相比,具有在温度25℃、频率1×105Hz下显示出1000MPa以上的储能模量的树脂层作为中间膜的实施例1~3的夹层玻璃显示出特别优异的耐崩裂性。
符号说明
1-夹层玻璃,2-夹层玻璃的中间膜用膜材料,5-中间膜,11、12-玻璃板,21、22-基材膜。
Claims (3)
1.一种车辆用夹层玻璃,其具备:
对置的两张玻璃板;及
中间膜,配置于所述两张玻璃板之间,
所述中间膜具有在温度25℃、频率1×105Hz下显示出1000MPa以上的储能模量的树脂层。
2.根据权利要求1所述的车辆用夹层玻璃,其中,
所述两张玻璃板的厚度不同,所述树脂层与更厚的所述玻璃板相邻。
3.根据权利要求1或2所述的车辆用夹层玻璃,其为汽车用前窗玻璃。
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PCT/JP2019/046442 WO2020111153A1 (ja) | 2018-11-30 | 2019-11-27 | 車両用合わせガラス |
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JPWO2020111153A1 (ja) | 2021-11-04 |
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