CN111576079A - 一种导电性炭纸及其制备方法 - Google Patents

一种导电性炭纸及其制备方法 Download PDF

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Publication number
CN111576079A
CN111576079A CN202010388653.7A CN202010388653A CN111576079A CN 111576079 A CN111576079 A CN 111576079A CN 202010388653 A CN202010388653 A CN 202010388653A CN 111576079 A CN111576079 A CN 111576079A
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paper
carbon
conductive carbon
porosity
carbon paper
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CN111576079B (zh
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吴刚平
刘玉婷
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/36—Inorganic fibres or flakes
    • D21H13/46—Non-siliceous fibres, e.g. from metal oxides
    • D21H13/50—Carbon fibres
    • 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
    • B32B29/00—Layered products comprising a layer of paper or cardboard
    • B32B29/002—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B29/005—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material next to another layer of paper or cardboard layer
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
    • C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
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    • D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • D—TEXTILES; PAPER
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    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
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    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/07—Nitrogen-containing compounds
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    • D21H17/03—Non-macromolecular organic compounds
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    • D21H17/11—Halides
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    • D21H17/03—Non-macromolecular organic compounds
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    • D21H17/14—Carboxylic acids; Derivatives thereof
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    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
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    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
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    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/35—Polyalkenes, e.g. polystyrene
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    • D21H17/36—Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
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    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
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Abstract

本发明属于导电性材料制备方法技术领域，具体涉及一种导电性炭纸及其制备方法。本发明导电性炭纸由2～10层孔隙率为10～80％的单层碳纤维纸构成，其中最外侧一面的单层碳纤维纸的孔隙率记为A，另一面最外侧的单层碳纤维纸的孔隙率记为B，其中A、B单位为％，导电性炭纸的总厚度记为L，其中L单位为μm，三者须符合如下关系：0.2≤│A‑B│/L≤0.8。本发明通过将含有分散剂、短切碳纤维、纳米碳纤维的混合物置于水中，打浆使得碳纤维和纳米碳纤维分散均匀，形成悬浮液；采用常规湿法抄纸技术将悬浮液进行制造，形成碳纤维原纸；浸渍粘结剂，并烘干，然后进行炭化，得到导电性炭纸。

Description

一种导电性炭纸及其制备方法
技术领域
本发明属于导电性材料制备方法技术领域，具体涉及一种导电性炭纸及其制备方法。
背景技术
质子交换膜氢燃料电池的气体扩散层需同时具有集电、气体传输、气流分配等功能。由此，构成气体扩散层的碳纤维纸层材料中，要求同时具有高导电性、高气体扩散性、高气体分配性等性能。
作为质子交换膜燃料电池的气体扩散层用炭纸，日本公开特许专利第6-20710号公报记载，将短切碳纤维随机分散形成碳纤维纸，并进而由炭素材料结合起来，形成具有多孔质结构的碳纤维纸材料。然而，该碳纤维纸材料难以显著体现出对气流分配的能力。
另一方面，作为质子交换膜燃料电池的气体扩散层用炭纸，其一面与具有气体传输流路的双极板相结合，另一面与催化剂层相结合。因此，作为燃料电池用气体扩散层的导电基材，除了上述要求的导电性、气体透过性、气体分配性等之外，还要求与催化剂层具有良好的的结合性。然而，传统的电极基材中，为了提高气体传输性能，炭纸的孔隙率提高，使得炭纸表面变得粗糙，与催化剂层的结合不良。
发明内容
针对上述问题本发明提供了一种导电性炭纸及其制备方法。
为了达到上述目的，本发明采用了下列技术方案：
一种导电性炭纸，所述导电性炭纸由2～10层孔隙率为10～80％的单层碳纤维纸构成，其中最外侧一面的单层碳纤维纸的孔隙率记为A，另一面最外侧的单层碳纤维纸的孔隙率记为B，其中A、B单位为％，导电性炭纸的总厚度记为L，其中L单位为μm，三者须符合如下关系：0.2≤│A-B│/L≤0.8。当│A-B│/L大于0.8时，由于炭纸两面的孔隙率差异过大，导致炭纸至少一面的平整度降低；当│A-B│/L小于0.2时，炭纸两面的孔隙率差异过小，无法发挥梯度分配气流的作用。
进一步，所述导电性炭纸为非对称的多孔质结构炭纸，导电性炭纸孔隙率高的一面用于与双极板接触，孔隙率低的一面用于与催化剂层接触且在其表面设有微孔层；炭纸按照从孔隙率从小到大或者从大到小的顺序依次排布。在使用时将孔隙率最大的一面与双极板相接触，保证气流在从大孔向小孔过渡的过程中实现气流的逐步均匀分配；将孔隙率最小的一面与催化剂层相接触，保证与催化剂层结合紧密。如果孔隙率不按从大到小或从小到大的顺序排列，将出现气流发生紊乱流动的现象。
再进一步，所述微孔层是聚四氟乙烯与炭素粒子的混合物。聚四氟乙烯使得微孔层总体上疏水性增强，有利于反应生成水的排放；而炭素粒子的加入使得微孔层的导电性提高，有利于电子传输。
一种导电性炭纸的制备方法，包括以下步骤：
步骤1，将含有分散剂、短切碳纤维和纳米碳纤维的混合物置于水中，打浆使得短切碳纤维和纳米碳纤维分散均匀，形成悬浮液；
步骤2，采用常规湿法抄纸技术将悬浮液进行制备，形成碳纤维原纸；
步骤3，将碳纤维原纸浸渍粘结剂，并烘干；
步骤4，将浸渍粘结剂烘干并经过热压的碳纤维原纸进行炭化，得到导电性炭纸。
进一步，所述步骤1中短切碳纤维的直径为2μm～15μm，长度为1mm～30mm。如短切碳纤维的直径小于2μm，将造成工艺过程复杂，导致生产成本增加；如短切碳纤维的直径大于15μm，将难以稳定制造。如短切碳纤维的长度小于1mm，将造成切丝过程的成本增加，而如短切碳纤维的长度超过30mm，将导致短切碳纤维难以均匀分散。
进一步，所述步骤1中纳米碳纤维的直径为20nm～200nm，长度为0.5μm～500μm。如纳米碳纤维的直径小于20nm，将造成抄纸过程中物料损失严重；如纳米碳纤维的直径超过200nm，将造成生产成本过高。如纳米碳纤维的长度小于0.5μm，将造成抄纸过程中物料流失严重；如纳米碳纤维的长度超过500μm，将造成抄纸过程中分散困难。
进一步，所述步骤1中分散剂是：十二烷基苯磺酸钠、酰基羟乙基磺酸钠、多聚磷酸酯、聚丙烯酸钠、N-烷基三甲基氯化铵、聚氧乙烯胺、聚乙烯亚胺、聚氧乙烯烷基酚、聚氧乙烯酯、聚乙烯醇、丙三醇、聚氧乙烯、聚丙烯酰胺、脂肪族聚氧乙烯醚、羧甲基纤维素、N-烷基甜菜碱、N-烷基氨基酸、咪唑啉羧酸盐中的一种或两种以上任意比例的混合物，主要作用是将短碳纤维进行均匀分散，使得可通过湿法抄纸工艺制成厚度均一的碳纤维纸。
进一步，所述步骤1中分散剂用量为水用量的0.01～2wt％。分散剂用量超过水用量2wt％，将造成分散剂使用过量，增加成本；而如果分散剂用量为水用量的0.01％，分散剂的效果不明显，不能有效将碳纤维分散。
进一步，所述步骤1中短切碳纤维与纳米碳纤维以任意比例混合，且短切碳纤维与纳米碳纤维的用量之和为水用量的0.01～0.5wt％。如短切碳纤维与纳米碳纤维的用量之和超过水用量的0.5wt％，短切碳纤维和纳米碳纤维将难以有效分散；如短切碳纤维与纳米碳纤维的用量之和小于水用量的0.01wt％，将造成抄纸运行成本明显增加。
进一步，所述步骤3中粘结剂为酚醛树脂、水解度为10～90％的聚丙烯腈树脂、壳聚糖、呋喃树脂、三聚氰胺、沥青、苯并噁嗪树脂中的一种或两种以上任意比例混合物的溶液，所述溶液的溶剂为水、甲醇或乙醇。选用这些粘结剂，一方面起到粘结相邻短碳纤维的作用，另一方面，也可使得在后期炭化过程中由树脂转化为炭素结构，提高碳纤维纸的导电性。
进一步，所述步骤3中粘结剂浓度为1～100g/L。粘结剂的浓度如果超过100g/L，将造成碳纤维纸中空孔结构被堵塞；如果小于1g/L，不能起到有效粘结短碳纤维的作用。
进一步，所述步骤3中烘干的烘干温度120℃，烘干时间为10min；所述步骤4的热压温度为120～200℃，压力为0.5～5Mpa；所述步骤4中炭化的最高炭化温度为1400～2200℃，炭化时间5s～20min。最高炭化温度如果超过2200℃，将造成能源的浪费，增加成本，而如果低于1400℃，则炭化不充分，粘结剂树脂不能充分转化为炭素结构；炭化时间如果超过20min，造成生产效率下降，而如果小于5s，无法有效炭化粘结剂树脂。
一种导电性炭纸的应用，应用于质子交换膜氢燃料气体扩散层的电极基材。炭纸经进一步疏水改性、设置微孔层后，可作为气体扩散层电极材料使用，因而炭纸是气体扩散层的电极基材。
与现有技术相比本发明具有以下优点：
本发明一方面满足氢燃料电池中作为气体扩散层材料要求的高导电性、高气体扩散性、高气流分配性，另一方面满足与催化剂层结合良好的要求。
传统炭纸中孔隙率基本相同，如果孔隙率过低，从双极板的气体流路传输的气体难以有效进入炭纸，存在侧漏风险；如果孔隙率过高，则炭纸的表面平整度整体下降，炭纸与催化剂层的结合不紧密，既存在气体侧漏的可能性，也不利于气流均匀分布进行催化剂层，还不利于反应产生电子的有效传输。本发明的材料结构可保证炭纸表面孔隙率高的一面与双极板相接触，可保证气体有效的传输进入炭纸，降低气体的入口压力；而在另一面，由于炭纸的孔隙率低，表面平整度高，使得炭纸与催化剂层可充分接触，有利于气流的均匀分配到催化剂层，并有效传输反应产生的电子。
具体实施方式
[聚丙烯腈水解度的测试方法]
利用聚丙烯腈水解前和水解后含氮量的变化，可以确定聚丙烯腈的水解度(DH)，设N0为水解前聚丙烯腈的含氮量，Nt是水解后聚丙烯腈的含氮量，则聚丙烯腈的水解度DH可由下式计算得到：
Figure BDA0002484818670000051
其中含氮量的变化有元素分析法得到。
实施例1
一种导电性炭纸，所述导电性炭纸由2～10层孔隙率为10～80％的单层碳纤维纸构成，其中最外侧一面的单层碳纤维纸的孔隙率记为A，另一面最外侧的单层碳纤维纸的孔隙率记为B，其中A、B单位为％，导电性炭纸的总厚度记为L，其中L单位为μm,三者须符合如下关系：0.2≤│A-B│/L≤0.8。
所述导电性炭纸为非对称的多孔质结构炭纸，导电性炭纸孔隙率高的一面用于与双极板接触，孔隙率低的一面用于与催化剂层接触且在其表面设有微孔层。炭纸按照从孔隙率从小到大或者从大到小的顺序依次排布。
一种导电性炭纸的制备方法，包括以下步骤：
在1000mL去离子水中，加入1g羟甲基纤维素、0.05g短切碳纤维(长度6mm、直径5μm)及0.05g纳米碳纤维(直径范围为20-50nm，长度范围为1～200μm)，通过打浆使得碳纤维和纳米碳纤维分散均匀，形成稳定悬浮液，其中含有0.1wt％羟甲基纤维素、0.005wt％的短切碳纤维(长度6mm、直径5μm)、0.005wt％的碳纳米纤维(直径范围为20-50nm,长度范围为1～200μm)；采用常规湿法抄纸技术将悬浮液进行抄纸制造，得到碳纤维原纸。
将碳纤维原纸10张浸渍5g/L酚醛树脂的甲醇溶液，并在120℃下烘干，得到不同孔隙率碳纤维原纸。按照孔隙率由大致小顺序进行叠层放置，并在热压机上进行固化处理，温度160℃，压力0.2MPa，时间10min。将固化后的碳纤维原纸在氮气气氛保护下进行炭化，升温速度10℃/min，炭化温度1400℃，时间20min，得到导电性炭纸。
将炭纸在20％聚四氟乙烯乳液中浸润，并在120℃下烘干，后将炭纸放入马弗炉中在350℃下进行热处理。将10％聚四氟乙烯与载炭量5mg/cm2炭黑调制成乳液，将炭纸进行单面涂层制备微孔层，并在120℃下烘干，后将炭纸放入马弗炉在350℃下中进行热处理，形成导电性炭纸。
将得到的炭纸进行扫描电子显微镜观测，通过图像分析确定炭纸两侧孔隙率(A、B)，采用测厚仪得到炭纸的总厚度(L)，计算其│A-B│/L数值列于表2。
将自制导电性炭纸，在条件固定的燃料电池测试系统中进行单电池性能测试，得到功率密度参数，测试结果列于表2。
实施例2～10
一种导电性炭纸，所述导电性炭纸由2～10层孔隙率为10～80％的单层碳纤维纸构成，其中最外侧一面的单层碳纤维纸的孔隙率记为A，另一面最外侧的单层碳纤维纸的孔隙率记为B，其中A、B单位为％，导电性炭纸的总厚度记为L，其中L单位为μm，三者须符合如下关系：0.2≤│A-B│/L≤0.8。
所述导电性炭纸为非对称的多孔质结构炭纸，导电性炭纸孔隙率高的一面用于与双极板接触，孔隙率低的一面用于与催化剂层接触且在其表面设有微孔层。炭纸按照从孔隙率从小到大或者从大到小的顺序依次排布。
一种导电性炭纸的制备方法，改变工艺参数列于表1，其余制备过程均参照实施例1中方法进行。
将得到的炭纸进行扫描电子显微镜观测，通过图像分析确定炭纸两侧孔隙率(A、B)，采用测厚仪得到炭纸的总厚度(L)，计算其│A-B│/L数值列于表2。
将自制导电性炭纸，在条件固定的燃料电池测试系统中进行单电池性能测试，得到功率密度参数，测试结果列于表2。
比较例
在1000ml去离子水中加入10g十二烷基苯磺酸钠、5g长度为6mm的短切碳纤维，通过打浆使得短切碳纤维分散均匀，形成稳定悬浮液。采用常规湿法抄纸技术将悬浮液进行抄纸制造，得到碳纤维原纸。
将单张碳纤维浸渍5g/L酚醛树脂的甲醇溶液，并在120℃下烘干，并在热压机上进行固化处理，温度160℃，压力0.2MPa，时间10min。将固化后的碳纤维原纸在氮气气氛保护下进行炭化，升温速度10℃/min，炭化温度1500℃，时间20min，得到导电性炭纸。
将炭纸在20％聚四氟乙烯乳液中浸润，并在120℃下烘干，后将炭纸放入马弗炉中在350℃下进行热处理。将10％聚四氟乙烯与载炭量1.5mg/cm2炭黑调制成乳液，将炭纸在铺布机进行单面涂层制备微孔层，并在120℃下烘干，后将炭纸放入马弗炉在350℃下中进行热处理，形成导电性炭纸。
将得到的炭纸进行扫描电子显微镜观测，通过图像分析确定炭纸两侧孔隙率(A、B)，采用测厚仪得到炭纸的总厚度(L)，计算其│A-B│/L数值列于表2。
将自制导电性炭纸，在条件固定的燃料电池测试系统中进行单电池性能测试，得到功率密度参数，测试结果列于表2。
表1
Figure BDA0002484818670000091
表2
Figure BDA0002484818670000101
本发明说明书中未作详细描述的内容属于本领域专业技术人员公知的现有技术。尽管上面对本发明说明性的具体实施方式进行了描述，以便于本技术领的技术人员理解本发明，但应该清楚，本发明不限于具体实施方式的范围，对本技术领域的普通技术人员来讲，只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内，这些变化是显而易见的，一切利用本发明构思的发明创造均在保护之列。

Claims (10)

1.一种导电性炭纸，其特征在于：所述导电性炭纸由2～10层孔隙率为10～80％的单层碳纤维纸构成，其中最外侧一面的单层碳纤维纸的孔隙率记为A，另一面最外侧的单层碳纤维纸的孔隙率记为B，其中A、B单位为％，导电性炭纸的总厚度记为L，其中L单位为μm，三者须符合如下关系：0.2≤│A-B│/L≤0.8。
2.根据权利要求1所述的一种导电性炭纸，其特征在于：所述导电性炭纸为非对称的多孔质结构炭纸，导电性炭纸孔隙率高的一面用于与双极板接触，孔隙率低的一面用于与催化剂层接触且在其表面设有微孔层；炭纸按照从孔隙率从小到大或者从大到小的顺序依次排布。
3.一种导电性炭纸的制备方法，其特征在于：包括以下步骤：
步骤1，将含有分散剂、短切碳纤维和纳米碳纤维的混合物置于水中，打浆使得短切碳纤维和纳米碳纤维分散均匀，形成悬浮液；
步骤2，采用常规湿法抄纸技术将悬浮液进行制备，形成碳纤维原纸；
步骤3，将碳纤维原纸浸渍粘结剂，并烘干；
步骤4，将浸渍粘结剂后烘干并经过热压的碳纤维原纸进行炭化，得到导电性炭纸。
4.根据权利要求3所述的一种导电性炭纸的制备方法，其特征在于：所述步骤1中短切碳纤维的直径为2μm～15μm，长度为1mm～30mm。
5.根据权利要求3所述的一种导电性炭纸的制备方法，其特征在于：所述步骤1中纳米碳纤维的直径为20nm～200nm，长度为0.5μm～500μm。
6.根据权利要求3所述的一种导电性炭纸的制备方法，其特征在于：所述步骤1中分散剂是：十二烷基苯磺酸钠、酰基羟乙基磺酸钠、多聚磷酸酯、聚丙烯酸钠、N-烷基三甲基氯化铵、聚氧乙烯胺、聚乙烯亚胺、聚氧乙烯烷基酚、聚氧乙烯酯、聚乙烯醇、聚乙二醇、丙三醇、聚氧乙烯、聚丙烯酰胺、脂肪族聚氧乙烯醚、羧甲基纤维素、N-烷基甜菜碱、N-烷基氨基酸、咪唑啉羧酸盐中的一种或两种以上任意比例的混合物。
7.根据权利要求3所述的一种导电性炭纸的制备方法，其特征在于：所述步骤1中分散剂的用量为水用量的0.01～2wt％，短切碳纤维与纳米碳纤维以任意比例混合，且短切碳纤维与纳米碳纤维用量之和为水用量的0.01～0.5wt％。
8.根据权利要求3所述的一种导电性炭纸的制造方法，其特征在于：所述步骤3中粘结剂为酚醛树脂、水解度为10～90％的聚丙烯腈树脂、壳聚糖、呋喃树脂、三聚氰胺、沥青、苯并噁嗪树脂中的一种或两种以上任意比例混合物的溶液，所述溶液的溶剂为水、甲醇或乙醇。
9.根据权利要求3所述的一种导电性炭纸的制造方法，其特征在于：所述步骤3中粘结剂浓度为1～100g/L。
10.根据权利要求3所述的一种导电性炭纸的制造方法，其特征在于：所述步骤3中烘干的烘干温度120℃，烘干时间为10min；所述步骤4热压的热压温度为120～200℃，热压压力为0.5～5Mpa；所述步骤4中炭化的炭化温度为1400～2200℃，炭化时间5s～20min。
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