TW201437301A - 透明碳納米管高分子複合導電墨水及其製備方法 - Google Patents
透明碳納米管高分子複合導電墨水及其製備方法 Download PDFInfo
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- TW201437301A TW201437301A TW103110032A TW103110032A TW201437301A TW 201437301 A TW201437301 A TW 201437301A TW 103110032 A TW103110032 A TW 103110032A TW 103110032 A TW103110032 A TW 103110032A TW 201437301 A TW201437301 A TW 201437301A
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Abstract
本發明涉及透明碳納米管高分子複合導電墨水及其製備方法。該導電墨水由改性後的碳納米管、導電高分子、水溶性高分子助溶劑、高分子改性助劑、表面活性劑和去離子水組成，且通過溶液的共混工藝技術，實現了碳納米管與導電高分子溶液的均勻分散，製備的墨水穩定性和再分散性良好。本發明可以在室溫條件下，採用spin coating、噴墨列印等設備製備精細的電極圖案，也可以通過光刻工藝實現精細的電極圖案製備，也可配製成光刻型的導電墨水，實現微細結構電極圖案的一次性製備。該墨水可應用於柔性OLED顯示器件、太陽能電池、液晶顯示，觸控式螢幕面板等器件中的極透明電極材料，與透明高分子基底相容性好，附著力強，確保柔性電極的使用壽命。
Description
本發明涉及有機電致發光器件領域，特別是涉及一種透明電極用透明碳納米管高分子複合導電墨水及其製備方法。
在液晶面板、OLED面板、觸控式螢幕、電子紙、太陽能電池等顯示器件和光伏器件中，透明電極都是不可缺少的部分。氧化銦錫(ITO)在玻璃基底上形成ITO薄膜顯示出優異的透光性和導電性，因此目前其在商業化透明電極的應用領域裡佔有主導地位。但隨著科技的發展及透明電極應用領域的多元化，透明電極必須具備低方阻，可見光範圍內良好的透過率、柔性、可實現大面積精細塗布成膜的簡單操作工藝等要求。這使得ITO(氧化銦錫)薄膜的拓展應用中存在技術上難以克服的問題。銦(In)是稀有元素，世界儲存量較少而且薄膜中In2O3的含量比較高，所以製備成本較高；由於ITO薄膜比較脆，在經過週期性多次彎曲或者壓縮後，容易產生裂縫，致使導電性失效。當ITO薄膜低溫沉積在相匹配的塑膠襯底時，膜層表現出相對高的表面電阻和粗糙度。因此，開發新型柔性透明電極材料來替代ITO電極是電子顯示領域和光伏等應用領域發展所必須解決技術難點。
碳納米管是一種具有典型的層狀中空結構特徵的碳材料,構成碳納米管的管身由六邊形石墨碳環結構單元組成, 是一種具有特殊結構（徑向尺寸為納米量級，軸向尺寸為微米量級）的一維量子材料。它的管壁構成主要為數層到數十層的同軸圓管。層與層之間保持固定的距離，約為0.34nm，直徑一般為2～20nm 。碳納米管上碳原子的P電子形成大範圍的離域π鍵，由於共軛效應顯著，碳納米管具有一些特殊的電學性質。由於碳納米管的結構與石墨的片層結構相同，所以具有很好的電學性能。 碳納米管材料因為其高電子遷移率，低電阻率及高透明度，已被科研和產業界認定為可代替ITO的透明電極。
碳納米管與導電材料製成複合層，可增加透明電極的導電性能，現在的方法一般是將碳納米管與導電材料製成混合液然後再噴塗，或是印刷在電極上，但由於碳納米管結構的特殊性，跟其它物質的相容性較差，混合液中碳納米管的分散性較差，而且混合液不穩定，且容易沉積。
本發明開發了一種新型的透明碳納米管高分子導電墨水，此墨水採用改性的碳納米管及導電高分子為原材料，採用特選的助溶劑，且通過溶液的共混工藝技術，實現了碳納米管與導電高分子溶液的均勻分散，製備的墨水穩定性和再分散性良好。
本發明還提供該透明碳納米管高分子導電墨水的製備方法。
透明碳納米管高分子導電墨水，其組分及其重量份如下： 1、改性後的碳納米管 0.01%-1%， 2、導電高分子 0.17%-2%， 3、水溶性高分子助溶劑 0.43%- 5% ， 4、表面活性劑 0.01%-0.05%， 5、高分子改性助劑 0.037%-0.44%， 6、去離子水 加至100%，
所述改性後的碳納米管採用下述方法製成：在碳納米管中加入30% HNO3溶液，通過超音波分散40min後，在50-70℃攪拌30min，用200μm的多孔濾膜過濾，清洗至中性，於100℃下烘乾，得到純化的改性後的碳納米管。
所述碳納米管為單壁碳納米管、雙壁碳納米管或多壁碳納米管粉體。
所述導電高分子為聚苯胺、聚3， 4-乙撐二氧噻吩、聚乙炔或聚吡咯。
所述相應的導電高分子助溶劑為聚苯乙烯磺酸鹽、樟腦磺酸、十二烷基苯磺酸、十六烷基苯磺酸或萘磺酸。
所述高分子改性助劑為：丙二醇、丙三醇、乙二醇丁醚、山梨醇、二甲基亞碸、N-N二甲基甲醯胺中的一種或幾種。
所述表面活性劑為十二烷基苯磺酸鈉或聚吡咯烷酮。
所述導電高分子為聚3,4-乙撐二氧噻吩，導電高分子助溶劑為聚苯乙烯磺酸鈉，所述表面活性劑為聚吡咯烷酮。
該透明碳納米管高分子導電墨水的製備方法，採用如下步驟： 1) 碳納米管純化改性：在碳納米管中加入30% HNO3溶液，通過超音波分散40min後，在50-70℃攪拌30min，用200μm的多孔濾膜過濾，清洗至中性。於100℃下烘乾，得到純化的改性後的碳納米管； 2) 將一定量的純化的改性後的碳納米管與表面活性劑混合溶解在一定量的水中，利用超音波分散儀和機械攪拌的方法進行充分分散，所得分散液經過200μm的過孔濾膜進行多次過濾，所得的濾液為碳納米管分散液； 3) 導電高分子：導電高分子助溶劑高分子體改性：將一定量的高分子改性助劑加入導電高分子：導電高分子助溶劑中，通過超音波分散和機械攪拌，形成澄清的溶液，溶液經過200μm的過孔濾膜進行多次過濾； 4) 將步驟2和步驟3所得的溶液進行共混，通過超音波和機械攪拌的方法形成穩定均勻的透明碳納米管高分子導電墨水。
所述導電高分子：導電高分子助溶劑為聚3， 4-乙撐二氧噻吩（PEDOT）：聚苯乙烯磺酸鈉（PSS）。
本發明配方中除了基本的改性後的碳納米管、導電高分子和去離子水外，另加入了導電高分子助溶劑，以及高分子改性助劑和表面活性劑，使該碳納米管的分散性能顯著提高，同時該墨水的穩定性好和再分散性好。
碳納米管作為導電薄膜的導電傳輸材料，其在導電高分子體系中的分散至關重要。但是由於碳納米管表面張力較大，容易團聚形成顆粒狀。由此，碳納米管較均勻的分散在此墨水體系中非常關鍵。本專利技術採用酸化的方法，去除了碳納米管表面的無定形態碳，同時也在碳納米管的表面嫁接了如OH、COOH類官能團，降低了碳納米管的團聚，增加了碳納米管的溶解性。並且在表面活性劑的對碳納米管表面張力的調整下，可增加碳納米管在墨水體系的穩定分散性。
導電高分子本身是難溶於水的物質，在高分子助溶劑的鍵合作用下，可形成一種可溶解的溶液體系。為調整其導電特性，可加入一些高熔點的物質來增強其導電性能即導電助劑。
本發明開發了一種新型的透明碳納米管高分子導電墨水，此墨水採用改性的碳納米管及導電高分子為原材料，通過溶液的共混工藝技術，實現了碳納米管與導電高分子溶液的均勻分散，製備的墨水穩定性和再分散性良好。該透明的碳納米管高分子導電墨水，可以在室溫條件下，採用spin coating、噴墨列印等設備製備精細的電極圖案，也可以通過光刻工藝實現精細的電極圖案製備，也可配製成光刻型的導電墨水，實現微細結構電極圖案的一次性製備。
該透明CNT墨水可應用於柔性OLED顯示器件、太陽能電池、液晶顯示，觸控式螢幕面板等器件中的極透明電極材料，與透明高分子基底相容性好，附著力強，確保柔性電極的使用壽命。
下面結合實施例對本發明做進一步的詳細說明。
實施例 1 ：改性後的碳納米管 0.05% 聚3， 4-乙撐二氧噻吩PEDOT 1% 聚苯乙烯磺酸鈉PSS 1% PVP 0.03% 丙三醇 0.08% 二甲基亞碸 0.08% 乙二醇丁醚 0.03% 水 97.8%
製備方法： 工藝步驟： 1) 碳納米管純化改性：在碳納米管中加入30% HNO3溶液，通過超音波分散40min後，在50-70℃攪拌30min，用200μm的多孔濾膜過濾，清洗至中性。於100℃下烘乾，得到純化的碳納米管。 2) 將一定量的純化的碳納米管與表面活性劑PVP混合溶解在一定量的水中，利用超音波分散儀和機械攪拌的放射進行充分分散，所得分散液經過200μm的過孔濾膜進行多次過濾。所得的濾液為碳納米管分散液。 3) PEDOT：PSS高分子體改性。將一定量的高分子改性助劑加入PEDOT：PSS溶液中。通過超音波分散和機械攪拌，形成澄清的藍色溶液。溶液經過200μm的過孔濾膜進行多次過濾。 4) 按照一定比例將步驟2和步驟3所得的溶液進行共混，通過超音波和機械攪拌的方法形成穩定均勻的透明碳納米管高分子複合導電墨水製備。
實施例 2 ：改性後的碳納米管 0.05% 聚3， 4-乙撐二氧噻吩PEDOT 0.8% 聚苯乙烯磺酸鈉PSS 1% PVP 0.05%% 山梨醇 0.12% 二甲基亞碸 0.08% 乙二醇丁醚 0.025% 水 97%
製備方法：同實施例1。
透明的碳納米管高分子導電墨水，可以在室溫條件下，採用spin coating、噴墨列印等設備製備精細的電極圖案，也可以通過光刻工藝實現精細的電極圖案製備，也可配製成光刻型的導電墨水，實現微細結構電極圖案的一次性製備。
實驗例：將實施例1的導電墨水在電子玻璃基底上旋塗導電膜。見圖1。實施工藝：轉速3000rpm，時間30s， 烘烤溫度120℃，烘烤時間20min。
所得單層膜厚度為19-23nm，三層膜厚度為55-60nm，在300-600nm波長範圍內，光學透過率（相對於基底）均大於90%。三層薄膜方阻達到150-200Ω/□。見表1、圖2。
表1 實施例1所製備薄膜導電性及薄膜厚度測試結果
[圖1] 係碳納米管（CNT）及CNT/PEDOT：PSS （實施例1）薄膜的表面形貌測試圖；以及 [圖2]係實施例1製備薄膜光學透過率測試結果。
Claims (9)
- 一種透明碳納米管高分子導電墨水，其組分及其重量份如下： 1) 改性後的碳納米管 0.01%-1%， 2) 導電高分子 0.17%-2%， 3) 水溶性高分子助溶劑 0.43%- 5%， 4) 表面活性劑 0.01%-0.05%， 5) 高分子改性助劑 0.037%-0.44%， 6) 去離子水 加至100%， 所述改性後的碳納米管採用下述方法製成：在碳納米管中加入30%HNO3溶液，通過超音波分散40min後，在50-70℃攪拌30min，用200μm的多孔濾膜過濾，清洗至中性，於100℃下烘乾，得到純化的改性後的碳納米管。
- 如申請專利範圍第1項所述的透明碳納米管高分子導電墨水，所述碳納米管為單壁碳納米管、雙壁碳納米管或多壁碳納米管粉體。
- 如申請專利範圍第1項所述的透明碳納米管高分子導電墨水，所述導電高分子為聚苯胺、聚3， 4-乙撐二氧噻吩、聚乙炔或聚吡咯，所述相應的導電高分子助溶劑為聚苯乙烯磺酸鹽、樟腦磺酸、十二烷基苯磺酸、十六烷基苯磺酸或萘磺酸。
- 如申請專利範圍第3項所述的透明碳納米管高分子導電墨水，所述表面活性劑為十二烷基苯磺酸鈉或聚吡咯烷酮。
- 如申請專利範圍第4項所述的透明碳納米管高分子導電墨水，所述導電高分子為聚3， 4-乙撐二氧噻吩，導電高分子助溶劑為聚苯乙烯磺酸鈉，所述表面活性劑為聚吡咯烷酮。
- 如申請專利範圍第1項所述的透明碳納米管高分子導電墨水，所述高分子改性助劑為：丙二醇、丙三醇、乙二醇丁醚、山梨醇、二甲基亞碸、N-N二甲基甲醯胺中的一種或幾種。
- 如申請專利範圍第1項所述的透明碳納米管高分子導電墨水，所述導電高分子為聚3,4-乙撐二氧噻吩，導電高分子助溶劑為聚苯乙烯磺酸鈉，所述表面活性劑為聚吡咯烷酮。
- 一種製備如申請專利範圍第1~7項中任一項之透明碳納米管高分子複合導電墨水的製備方法，採用如下步驟： 1) 碳納米管純化改性：在碳納米管中加入30% HNO3溶液，通過超音波分散40min後，在50-70℃攪拌30min，用200μm的多孔濾膜過濾，清洗至中性。於100℃下烘乾，得到純化的改性後的碳納米管； 2) 將一定量的純化的改性後的碳納米管與表面活性劑混合溶解在一定量的水中，利用超音波分散儀和機械攪拌的方法進行充分分散，所得分散液經過200μm的過孔濾膜進行多次過濾。所得的濾液為碳納米管分散液； 3) 導電高分子：導電高分子助溶劑高分子體改性：將一定量的高分子改性助劑加入導電高分子：導電高分子助溶劑中，通過超音波分散和機械攪拌，形成澄清的溶液，溶液經過200μm的過孔濾膜進行多次過濾； 4) 將步驟2和步驟3所得的溶液進行共混，通過超音波和機械攪拌的方法形成穩定均勻的透明碳納米管高分子導電墨水。
- 如申請專利範圍第8項所述的方法，所述導電高分子：導電高分子助溶劑為聚3， 4-乙撐二氧噻吩：聚苯乙烯磺酸鈉。
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| CN109021711B (zh) * | 2018-08-02 | 2021-06-18 | 苏州蓝沛光电科技有限公司 | 一种用于制造含金属网格结构触摸屏的油墨 |
| CN109266081A (zh) * | 2018-09-11 | 2019-01-25 | 东莞市鼎力薄膜科技有限公司 | 高效防静电液及其制备方法 |
| CN109627849B (zh) * | 2018-11-22 | 2021-09-21 | 武汉纺织大学 | 一种碳纳米管/聚吡咯纳米管复合电子墨水及其制备方法 |
| CN111446366B (zh) * | 2019-01-17 | 2021-09-24 | 中国科学院金属研究所 | 凝胶型聚合物电解质修饰石墨烯、碳纳米管或其复合透明导电膜的方法与应用 |
| KR102125401B1 (ko) * | 2019-01-25 | 2020-06-23 | (주)수양켐텍 | 인시튜(In-situ) 공정 기반의 탄소나노소재/PEDOT:PSS 하이브리드 전도성 고분자 제조방법, 이로부터 제조된 하이브리드 전도성 고분자 및 이를 이용한 대전방지 코팅액 |
| CN109830512A (zh) * | 2019-01-30 | 2019-05-31 | 合肥鑫晟光电科技有限公司 | 显示基板、显示基板的制备方法、显示装置 |
| CN113646177B (zh) * | 2019-03-29 | 2023-05-09 | 富士胶片株式会社 | 喷墨油墨、红外线吸收图像形成方法及记录物 |
| CN110611029B (zh) * | 2019-09-04 | 2022-01-18 | 北京华碳元芯电子科技有限责任公司 | 一种印刷法制备碳纳米管薄膜的方法 |
| KR102294709B1 (ko) * | 2019-12-05 | 2021-08-27 | (주)수양켐텍 | 분산안정성과 높은 전도성을 갖는 전도성 고분자 제조방법, 이로부터 제조된 전도성 고분자 및 이를 이용한 대전방지 코팅액 |
| CN111073395A (zh) * | 2019-12-27 | 2020-04-28 | 新奥石墨烯技术有限公司 | 一种透明电热油墨及其制备方法、电热膜 |
| CN111205498A (zh) * | 2020-03-20 | 2020-05-29 | 桂林电子科技大学 | 一种静电式导电油墨/聚丙烯集尘板的制备方法 |
| CN111292874B (zh) * | 2020-03-23 | 2022-10-14 | 智能容电(北京)科技有限公司 | 一种高导电屈服电极材料及其制备方法 |
| CN112341865B (zh) * | 2020-10-27 | 2022-04-22 | 华南理工大学 | 一种cnt:snc:pedot三元水性导电油墨及其制备方法 |
| CN115044949B (zh) * | 2022-06-09 | 2023-10-20 | 合肥工业大学 | 一种改性有机防腐涂层的制备装置及方法 |
| WO2024035559A1 (en) * | 2022-08-09 | 2024-02-15 | ExxonMobil Technology and Engineering Company | Solvents for carbon nanotube dispersions |
| CN117586539B (zh) * | 2024-01-18 | 2024-05-14 | 成都飞机工业（集团）有限责任公司 | 一种高导电自支撑碳纳米管复合薄膜的制备方法 |
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| TWI419924B (zh) * | 2007-01-17 | 2013-12-21 | Arakawa Chem Ind | An organic solvent dispersion of a conductive polymer / dopant, and a composition containing the dispersion |
| US8414964B2 (en) * | 2007-09-28 | 2013-04-09 | Toray Industries, Inc. | Process for producing electrically conductive film |
| CN101486836A (zh) * | 2008-01-18 | 2009-07-22 | 郑州泰达电子材料科技有限公司 | 导电性高分子溶液、导电性高分子涂膜导电性高分子溶液的制备方法以及固体电解电容器 |
| JP5243067B2 (ja) * | 2008-03-10 | 2013-07-24 | 日機装株式会社 | 導電性ポリマーの導電性向上方法 |
| WO2010051102A2 (en) * | 2008-09-09 | 2010-05-06 | Sun Chemical Corporation | Carbon nanotube dispersions |
| WO2010030123A2 (ko) * | 2008-09-12 | 2010-03-18 | 주식회사 엘지화학 | 금속 나노벨트, 이의 제조 방법, 이를 포함하는 도전성 잉크 조성물 및 전도성 필름 |
| US20110248223A1 (en) * | 2008-12-31 | 2011-10-13 | Essilor International (Compagnie Generale D'optique) | Additives for Enhancing the Antistatic Properties of Conductive Polymer-Based Coatings |
| JP5393173B2 (ja) * | 2009-01-21 | 2014-01-22 | 信越ポリマー株式会社 | 導電性インク、透明導電層、及び入力デバイス |
| US20120015098A1 (en) * | 2010-07-14 | 2012-01-19 | Qian Cheng | Carbon nanotube based transparent conductive films and methods for preparing and patterning the same |
| JP5682887B2 (ja) * | 2010-11-02 | 2015-03-11 | 学校法人東京理科大学 | 導電性高分子ナノ微粒子分散溶液、当該分散溶液を用いた導電薄膜及び導電薄膜の製造方法 |
| JP2012097219A (ja) * | 2010-11-04 | 2012-05-24 | Sony Corp | 導電性インク、導電性インクの製造方法および透明導電膜の製造方法 |
| US9803097B2 (en) * | 2012-10-29 | 2017-10-31 | 3M Innovative Properties Company | Conductive inks and conductive polymeric coatings |
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| WO2014146534A1 (zh) | 2014-09-25 |
| JP6244006B2 (ja) | 2017-12-06 |
| KR20160009544A (ko) | 2016-01-26 |
| HK1196974A1 (zh) | 2014-12-24 |
| JP2016519700A (ja) | 2016-07-07 |
| DE112014001525T5 (de) | 2015-12-03 |
| CN104059432B (zh) | 2016-01-06 |
| CN104059432A (zh) | 2014-09-24 |
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