CN114867797A - 基于银纳米粒子的油墨 - Google Patents
基于银纳米粒子的油墨 Download PDFInfo
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- CN114867797A CN114867797A CN202080085230.6A CN202080085230A CN114867797A CN 114867797 A CN114867797 A CN 114867797A CN 202080085230 A CN202080085230 A CN 202080085230A CN 114867797 A CN114867797 A CN 114867797A
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
本发明是有关于基于银纳米粒子的可热成型及/或可拉伸的油墨配方。具体地,本发明是有关于基于银纳米粒子、聚氨酯以及银、铜及/或镍金属微粒的油墨配方。
Description
技术领域
本发明是有关于基于银纳米粒子的可热成型及/或可拉伸的油墨配方。具体地,本发明是有关于基于银纳米粒子、聚氨酯以及银、铜及/或镍金属微粒的油墨配方,上述之油墨是稳定的,具有改善的导电性,可热成型及/或可拉伸,并且可有利地形成可拉伸及/或可形变的导电迹线,适用于可形变连接物,例如适用于置于被连接织物上的传感器,此种织物亦被称为智能织物,可应用于诸多领域,例如但不限于服装、保健、清洁技术、家具、土工织物及农业。
背景技术
在许多工业领域中,对于制造适用于可形变及/或弹性基材的导电迹线存在切实需求,以用于注塑(尤其是汽车)、织物或可形变连接物、传感器及生物传感器(敷料、化妆品贴片等)、RFID及NFC天线等各种应用,因此所有此等物体大多位于运动部件或物体上。
发明内容
根据本发明的基于导电纳米粒子的可热成型及/或可拉伸油墨可印刷在所有类型的基材上,由于形成适用于上述之基材的可拉伸及/或可变形导电迹线,因此可满足诸多任务业领域的要求。作为示例,可列举塑料、热塑性材料、硅酮化合物、含氟化合物,广义的具有弹性的任何材料、聚氨酯、PET、PEN、PC、复合材料、玻璃、环氧树脂、碳硅等。
采用根据本发明的基于导电纳米粒子的油墨制成的可热成型及/或可拉伸导电迹线,具有支持单次或重复形变的能力,同时充分保持其物理完整性及电学特性,特别是导电性。因此,请求保护之油墨具有诸多优点,其中作为非限制性示例可列举如下:
-退火更佳(沉积物均匀性);
-印刷过程中不产生气泡/泡沫;
-停留时间更长;
-与现有油墨相比,随时间推移的稳定性更高;
-溶剂及纳米粒子无毒;
-保留了纳米粒子的固有特性;特别是,
-在通常为150℃至300℃之间的退火温度下,导电性得到改善
-能够透过多种印刷方法进行印刷此一事实,其中作为示例可列举丝网印刷、苯胺印刷、喷墨、喷涂、涂层、镀膜、刻印等;及/或
-在塑料基材(PET、PC)上以及通常出现在热成型装置中的其他层(装饰油墨、电介质等)上的附着性更佳:
油墨:
透过能够形成可拉伸及/或可变形导电迹线的可热成型及/或可拉伸油墨,本发明可满足前述诸多目的,其中该油墨包含:
1、银纳米粒子,其含量至少为油墨重量的15%,较佳地,至少为油墨重量的20%,较佳地,含量小于油墨重量的45%,例如小于油墨重量的40%,
2、银、铜及/或镍金属微粒,其含量至少为油墨重量的15%,较佳地,至少为油墨重量的20%,较佳地,含量小于油墨重量的45%,例如小于油墨重量的40%,
3、沸点高于150℃的一元醇,其含量至少为油墨重量的20%,较佳地,至少为油墨重量的25%,较佳地,含量小于油墨重量的50%,例如小于油墨重量的45%,
4、成膜聚合物,其含量至少为油墨重量的0.5%,较佳地,至少为油墨重量的0.75%,较佳地,含量小于油墨重量的2%,例如小于油墨重量的1.25%,
5、多元醇及/或多元醇醚,其含量至少为油墨重量的1.5%,较佳地,至少为油墨重量的2%,较佳地,含量小于油墨重量的4%,例如小于油墨重量的3.5%,
6、纤维素化合物,其含量至少为油墨重量的0.4%,较佳地,至少为油墨重量的0.75%,较佳地,含量小于油墨重量的2%,例如小于油墨重量的1.5%,
上述化合物的总和至少占油墨重量的90%,较佳至少占油墨重量的95%,例如至少占油墨重量的99%。
·银纳米粒子
根据本发明的一种实施方式,请求保护之油墨中的银纳米粒子的粒度较佳地小于500nm,例如在1至250nm之间,较佳地在10至250nm之间,进一步较佳地在30至150nm之间。
本发明中提及的银纳米粒子的粒度分布可透过任何合适的方法来测量。例如,可有利地根据以下方法进行测量:使用马尔文公司的Nanosizer S型设备,其具有以下特征:
DLS(动态光散射)测量方法:
-容器类型:光学玻璃
-材料:银
-纳米粒子的折射率:0.54
-吸光度:0.001
-分散剂:环辛烷
-温度:20℃
-黏度:2.133
-分散剂的折射率:1.458
-一般选项:马克-霍温克参数
-分析模型:通用用途
-平衡:120s
-测量次数:4
D50是指数量50%的较小银纳米粒子的直径。该值被视为代表粒子的平均粒度。
根据本发明的一种实施改型,银纳米粒子为类球形及/或球形。在本发明以及下文中的权利要求中,术语“类球形”是指形状类似球形,但并不是完美的圆形(“准球形”),例如椭球形。
纳米粒子的形状及粒度可有利地透过显微镜拍摄的照片来识别,特别是透过符合下述说明的透射电子显微镜(TEM)型设备。采用Thermofisher Scientific公司的透射电子显微镜(TEM)型设备进行测量,其具有以下特征:
-TEM-BF(Bright Field–亮场)图像是在300kV下拍摄的,
-采用了用于低倍放大的50μm的物镜,没有高分辨率物镜,
-使用Digital Micrograph软件在TEM图像上进行尺寸测量,
-对代表大多数粒子的一定数量的粒子求平均值,例如20个粒子,如此便能确定纳米粒子的平均表面积、平均周长及/或平均直径。
因此,根据本发明的此一实施改型,纳米粒子是类球形的,并且透过该TEM鉴别,其特征较佳地在于纳米粒子的平均表面积在300至35000nm2之间,较佳地在700至20000nm2之间,及/或在于纳米粒子的平均周长在60至650nm之间,较佳地在90至500nm之间,及/或纳米粒子的平均直径在20至200nm之间,较佳地在30至150nm之间。
根据本发明一种实施改型,如果没有预先规定的形状,则银纳米粒子为丸状、棒状(长度L<200至300nm)、块状、片状或晶体的形式。
根据本发明的一种具体实施方式,透过物理合成或化学合成预先合成了银纳米粒子。在本发明的范围内,可采用任何物理或化学合成。在根据本发明的一种具体实施方式中,利用有机或无机银盐作为银前体,透过化学合成获得银纳米粒子。作为非限制性示例,可列举乙酸银、硝酸银、碳酸银、磷酸银、三氟化银、氯化银、高氯酸钾中的一种或它们的混合物。根据本发明的一种改型,前体为硝酸银及/或乙酸银。
根据本发明的一种具体实施方式,银纳米粒子的合成采用化学合成,存在分散剂时利用还原剂对银前体进行还原;此种还原可在不存在或存在溶剂的情况下进行。
因此,根据本发明使用的纳米粒子的特征为无论采用哪种合成方式(物理或化学),其D50之值较佳地在1至250nm之间;它们的特征还较佳地在于单分散(均匀)而没有聚集体。对于类球形银纳米粒子,亦可有利地采用30至150nm之间D50值。
本发明中提及的银纳米粒子的含量可透过任何合适的方法来测量。例如,可有利地根据以下方法进行测量:
-热解重量分析
-设备:TA Instrument公司的TGA Q50设备
-坩埚:氧化铝
-方法:斜面法
-测量范围:从室温到600℃
-升温速度:10℃/min。
·微粒
因此,根据本发明的油墨包含银、铜及/或镍金属微粒。此等微粒可呈球形、絮片状、针状/细线状/微线状及/或细丝状,并且较佳地粒度小于15μm,例如小于10μm,较佳小于5μm。微粒的平均表面积(根据上述TEM测量)在1至25μm2之间,较佳地在5至15μm2之间,及/或平均周长在3至20μm之间,较佳地在5至15μm之间,及/或平均直径在1至7μm之间,较佳地在1至5μm之间,因此有利地能够在本发明的范围内使用。
作为示例,金属微粒可由银、或铜-银混合物或镍-银混合物构成。具体地,此等微粒可具有铜芯及银壳,或者镍芯及银壳。如果是芯/壳粒子,则构成芯体的金属应占微粒总构成重量的85到95%。
根据本发明的一种实施方式,微粒由类球形微粒(较佳球形)及絮片状微粒的混合物构成。
根据本发明的一种实施方式,微粒由类球形微粒(较佳球形)及丝状、细线状、微线状及/或针状微粒的混合物构成。
本发明中提及的含有银的粒子含量可透过任何合适的方法来测量。例如,与银纳米粒子采用相同的方法。
根据本发明的一种实施方式,请求保护之油墨包含此等微粒的含量至少为油墨重量的15%,较佳至少为油墨重量的20%,并且较佳地含量小于油墨重量的45%,例如小于油墨重量的40%。
·成膜聚合物
因此,根据本发明的油墨包含成膜聚合物,具体包含合成的成膜聚合物,选自聚丙烯酸类、聚乙烯类、聚酯、聚硅氧烷及/或聚氨酯。该油墨具体地包含脂肪族聚氨酯,例如官能或非官能的饱和或不饱和脂肪族聚氨酯,例如半脂肪族聚氨酯,饱和或不饱和的官能或非官能半脂肪族聚氨酯。在不希望受限于该解释的情况下,申请人认为,该聚氨酯与油墨中的其他化合物结合,起到黏合剂的作用,以同时确保在沉积后具有良好附着性并形成弹性面。
·沸点高于150℃的一元醇
因此,根据本发明的油墨包含沸点高于150℃的一元醇;例如2,6-二甲基-4-庚醇及/或萜烯醇。根据本发明的油墨较佳地包含萜烯醇,选自薄荷醇、神经醇、桉树脑、熏衣草醇、肉豆蔻醇、萜品醇(α-、β-、γ-萜品醇及/或4-萜品醇;较佳地α-萜品醇)、异冰片醇、香茅醇、芳樟醇、冰片醇、香叶醇及/或两种或更多种上述之醇的混合物。
·多元醇及/或多元醇醚
因此,根据本发明的油墨包含多元醇及/或多元醇醚。该多元醇及/或多元醇醚的特征较佳地在于沸点低于260℃。可列举二醇(例如乙二醇、丙二醇、二甘醇、三亚甲基二醇、1,3-丁二醇、1,2-丁二醇、2,3-丁二醇、五亚甲基二醇、己烯乙二醇等),及/或二醇醚(例如乙二醇单醚或乙二醇二醚,作为示例可列举乙二醇单丙醚、乙二醇单丁醚、乙二醇单苯醚、丙烯乙二醇单苯醚、二乙二醇甲醚、二乙二醇乙醚、二乙二醇丙醚、二乙二醇丁醚(丁基卡必醇)、丙二醇单甲醚、丙二醇单丁醚、丙二醇单丙醚、乙二醇二甲醚、乙二醇二乙醚、乙二醇二丁醚、乙二醇二醚类(法语glymes)、二乙二醇二乙醚、二丁二醇二乙醚、二乙二醇二醚类(法语diglymes)、二乙二醇二乙醚(法语éthyle diglyme)、二乙二醇二丁醚(法语butylediglyme))及/或二醇醚乙酸酯(例如2-丁氧基乙酸酯、二乙二醇单乙基醚乙酸酯、二乙二醇丁醚乙酸酯、丙二醇甲醚乙酸酯)及/或两种或多种上述化合物的混合物。
·纤维素化合物
因此,根据本发明的油墨包含纤维素化合物。作为示例可列举烷基纤维素、羟烷基纤维素及羧烷基纤维素,较佳乙基纤维素。
根据本发明,20℃时,在40s-1的剪切速率下测得的油墨黏度通常在1000至100000mPa.s之间,较佳地在3000至30000mPa.s之间,例如在5000至20000mPa.s之间。
黏度可透过任何合适的方法来测量。例如,可有利地根据以下方法进行测量:
-设备:TA Instrument公司的AR-G2流变仪
-处理时间:100s-1下预剪切3分钟/平衡1分钟
-试验类型:剪切等级
-等级:40s-1、100s-1、1000s-1
-每级持续时间:5分钟
-模式:线性
-测量:每10秒钟
-温度:20℃
-曲线处理方法:牛顿法
-处理区域:整个曲线
因此,对于相关领域技术人员而言显而易见的是,在不脱离请求保护之本发明的应用范围的情况下,本发明允许采用诸多其他特定形式的实施方式。因此,所示实施方式应该被视作示例,但可在所附申请专利范围的范围所限定的领域内对本实施例进行修改。
附图说明
图1是热成型油墨338的图示。
图2是热成型油墨的表面平滑度的图示,图中从左到右分别为油墨303、315、338。
具体实施方式
现在将透过下面表格中列出的两种配方来说明本发明及其优点,其中表格中给出的数值对应于重量的百分浓度。
[表1]油墨21-4
[表2]油墨21-2
[表3]油墨21-11
请求保护之以及因此获得的油墨具有诸多优点,其中作为非限制性示例可列举如下:
-丝网印刷分辨率得到改善(线宽<50μm)
-热成型后导电性得到改善;及/或
-在塑料基材(PET、PC)上以及通常出现在热成型装置中其他层(装饰油墨、电介质等)上的附着性更佳:装饰油墨、电介质等;及/或
-对玻璃、ITO(掺杂锡的氧化铟)、PVDF(聚偏二氟乙烯)等基材有强附着性;及/或
-在高温下注入聚合物后在油墨沉积层上的附着力得以保持;及/或
-冷伸长至40%后具有良好导电性。
透过下面的实施例来说明本发明及其优点,该实施例说明了成膜聚合物及金属微粒对热成型后的油墨特性的共同作用。
[表4]
[表5]
[图1]为热成型油墨338的图示。
比较303及315的表面状态说明了油墨中存在聚氨酯的积极作用,使碎裂状态变为部分破裂状态。但是,为了获得平滑的表面状态并在热成型后保持良好的电学特性,有必要将聚氨酯的作用与微粒的作用结合起来,就如油墨338的结果所证明的那样。
[图2]为热成型油墨的表面平滑度的图示,图中从左到右分别为油墨303、315、338。
透过下面的实施例可说明本发明及其优点,该实施例说明了多形粒子混合物(不同粒度的细线体、球体)对于拉伸后的油墨特性的影响:
[表6]
[表7]
此等结果表明了存在多晶型粒子时的影响,该等多晶粒子使沉积物具有可拉伸性。此等粒子的含量达到30%,即使在伸长率达到40%时亦可保持良好的电学特性。
下表给出了油墨21-2及21-11的电学特性随着其经过的拉伸次数(伸长率30%)而变化的过程,其中[表8]中导线线宽为2mm,[表9]中导线线宽为250μm:
[表8]
[表9]
此等结果表明,即使有50次达到30%的伸长率,其电气性能仍然令人满意。发现电阻随着拉伸次数的增加而略有增加。
Claims (15)
1.一种可热成型及/或可拉伸的油墨,其中该油墨能够形成可拉伸及/或可变形导电迹线,该油墨包含重量比至少90%的以下多个化合物:
(1)银纳米粒子,其含量至少为该油墨重量的15%;
(2)银、铜及/或镍金属微粒,其含量至少为该油墨重量的15%;
(3)沸点高于150℃的一元醇,其含量至少为该油墨重量的20%;
(4)成膜聚合物,其含量至少为该油墨重量的0.5%;
(5)多元醇及/或多元醇醚,其含量至少为该油墨重量的1.5%;及
(6)纤维素化合物,其含量至少为该油墨重量的0.4%。
2.如权利要求1之油墨,其中该油墨包含:
(1)该银纳米粒子的含量至少为该油墨重量的20%并且小于该油墨重量的45%;
(2)该银、铜及/或镍金属微粒的含量至少为该油墨重量的20%,并且小于该油墨重量的45%;
(3)该一元醇的含量至少为该油墨重量的25%并且小于该油墨重量的50%;
(4)该成膜聚合物的含量至少为该油墨重量的0.75%并且小于该油墨重量的2%;
(5)该多元醇及/或多元醇醚的含量至少为该油墨重量的2%并且小于该油墨重量的4%;及
(6)该纤维素化合物的含量至少为该油墨重量的0.75%并且小于该油墨重量的2%。
3.如前述权利要求任一项之油墨,其中该油墨包含:
(1)该银纳米粒子的含量小于该油墨重量的40%;
(2)该银、铜及/或镍金属微粒的含量小于该油墨重量的40%;
(3)该一元醇的含量小于该油墨重量的45%;
(4)该成膜聚合物的含量小于该油墨重量的1.25%;
(5)该多元醇及/或多元醇醚的含量小于该油墨重量的3.5%;及
(6)该纤维素化合物的含量小于该油墨重量的1.5%。
4.如前述权利要求任一项所述之油墨,其中该等银纳米粒子为类球形,该类球形包含球形。
5.如前述权利要求任一项所述之油墨,其中该等银纳米粒子的平均直径在20至200nm之间,较佳地在30至150nm之间。
6.如前述权利要求任一项所述之油墨,其中该等银纳米粒子的D50之值在30至150nm之间。
7.如前述权利要求任一项所述之油墨,其中该等微粒的平均表面积在1至25μm2之间,较佳地在5至15μm2之间;及/或平均周长在3至20μm之间,较佳地在5至15μm之间;及/或该平均直径在1至7μm之间,较佳地在1至5μm之间。
8.如前述权利要求任一项之油墨,其中该成膜聚合物为合成聚合物,选自聚丙烯酸类、聚乙烯类、聚酯、聚硅氧烷及/或聚氨酯。
9.如权利要求8之油墨,其中该成膜聚合物为脂肪族聚氨酯,其中该脂肪族聚氨酯包含半脂肪族聚氨酯,其中该半脂肪族聚氨酯包含饱和或不饱和的官能或非官能半脂肪族聚氨酯。
10.如前述权利要求任一项之油墨,其中该沸点高于150℃的一元醇为2,6-二甲基-4-庚醇及/或萜烯醇。
11.如权利要求10之油墨,其中该萜烯醇为萜品醇。
12.如前述权利要求任一项之油墨,其中该多元醇及/或多元醇醚选自乙二醇及/或乙二醇醚。
13.如前述权利要求任一项之油墨,其中该多元醇及/或多元醇醚选自乙二醇、丙二醇、二甘醇、三亚甲基二醇、1,3-丁二醇、1,2-丁二醇、2,3-丁二醇、五亚甲基二醇、己烯乙二醇、乙二醇单丙醚、乙二醇单丁醚、乙二醇单苯醚、丙烯乙二醇单苯醚、二乙二醇甲醚、二乙二醇乙醚、二乙二醇丙醚、二乙二醇丁醚(丁基卡必醇)、丙二醇单甲醚、丙二醇单丁醚、丙二醇单丙醚、乙二醇二甲醚、乙二醇二乙醚、乙二醇二丁醚、乙二醇二醚类、二乙二醇二乙醚、二丁二醇二乙醚、二乙二醇二醚类、二乙二醇二乙醚、二乙二醇二丁醚。
14.如前述权利要求任一项之油墨,其中20℃时,在40s-1的剪切速率下测得的油墨黏度在1000至100000mPa.s之间,较佳地在3000至30000mPa.s之间,例如在5000至20000mPa.s之间。
15.一种将如前述权利要求任一项之油墨用于印刷/附着在玻璃、掺杂锡的氧化铟(ITO)或聚偏二氟乙烯(PVDF)基材上的用途。
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TW202122510A (zh) | 2021-06-16 |
WO2021115748A1 (fr) | 2021-06-17 |
JP2023505487A (ja) | 2023-02-09 |
CA3160185A1 (fr) | 2021-06-17 |
US20230348740A1 (en) | 2023-11-02 |
FR3104599B1 (fr) | 2021-11-26 |
BR112022011218A2 (pt) | 2022-08-23 |
FR3104599A1 (fr) | 2021-06-18 |
EP4073160A1 (fr) | 2022-10-19 |
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