CN107108227A - 石墨片及其制备方法 - Google Patents

石墨片及其制备方法 Download PDF

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CN107108227A
CN107108227A CN201680004414.9A CN201680004414A CN107108227A CN 107108227 A CN107108227 A CN 107108227A CN 201680004414 A CN201680004414 A CN 201680004414A CN 107108227 A CN107108227 A CN 107108227A
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graphite
graphite flake
substrate
flake
fiber
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CN107108227B (zh
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朴岐伦
甄明玉
金政圭
徐正斗
白种甲
朴钟辉
吴浚禄
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SKC Co Ltd
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SKC Co Ltd
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Abstract

本申请提供一种石墨片，该石墨片在水平和垂直方向的热扩散率之比为300或300以上。此外，本申请还提供了一种在垂直方向上的热扩散率为2.0mm2/s或2.0mm2/s以下的石墨片。该石墨片在水平和垂直方向上具有优异的导热性及柔韧性，并且制造成本低，因此具有经济优势。

Description

石墨片及其制备方法
技术领域
本申请涉及在水平/垂直方向上具有高热扩散率比且同时具有良好柔韧性的石墨片及其制备方法。
背景技术
近来，电子设备变得更轻、更薄、更短、更小，且多功能高度集成化，导致其热密度增加，因此，需要解决其热辐射问题。由于热辐射与设备的可靠性和寿命密切相关，因此是至关重要的。于是，现已有各种以散热垫、散热片、散热涂料等形式进行开发和销售的散热器了，它们可辅助或替代传统的散热装置，如散热风扇、散热销和散热管。
散热片可由石墨片、聚合物-陶瓷复合片、多层薄金属片等制成。石墨片轻薄而且具有与铜相当或甚至更高的导热性。因此，它们可用于等离子体电视的PDP中的电子电路板之间等。
制备膜状石墨的典型实例包括一种被称为“石墨膨胀法”的方法。在该方法中，通过将天然石墨浸入浓硫酸和浓醋酸的混合物中并将其快速加热来制备石墨。经洗涤除去酸之后，通过高压压制将由此获得的石墨成形为膜状。然而，由此制备的膜状石墨具有强度弱、其它物理性能不太好的缺点，并且任何残留酸的存在都会带来潜在的不利影响。
为了解决上述缺点，已经开发了通过对特定聚合物膜直接进行热处理的石墨化方法(以下称为“聚合物石墨化方法”)。该方法中使用的聚合物膜包括例如聚二唑、聚酰亚胺、聚亚苯基亚乙烯、聚苯并咪唑、聚苯并恶唑、聚噻唑和聚酰胺膜。聚合物石墨化方法与传统的石墨膨胀方法相比非常简单，其特征在于，其基本上不涉及杂质(如酸)，并且在该方法中产生的石墨具有接近单晶石墨的良好导热性或导电性(参见日本公开专利昭60-181129、平7-109171和昭61-275116)。
此外，在聚合物石墨化方法中，可向聚合物膜中添加碳纳米管等添加剂提高石墨的机械性能(参见日本专利第5275721号)。
然而，与石墨膨胀法相比，聚合物石墨化方法难以在厚膜中制备石墨。
尽管常规石墨片在水平方向上具有较高的热扩散率(或导热率)，但它们在垂直方向上具有较低的热扩散率并且价格昂贵。
发明内容
技术问题
本申请的目的是为了提供一种石墨片及其制备方法，通过降低垂直方向上的热扩散率和提高水平方向的热扩散率，该石墨片具有高的水平/垂直方向热扩散率之比。
本申请的另一个目的是为了提供一种具有高的水平/垂直方向热扩散率之比且同时具有良好的柔韧性的石墨片。
解决方案
本申请提供一种石墨片，该石墨片水平/垂直方向的热扩散率之比为300或300以上。
本申请提供一种石墨片，该石墨片在垂直方向上的热扩散率为2.0mm2/s或2.0mm2/s以下。
本申请提供一种石墨片的制备方法，包括：(1)提供基底，该基底包含天然纤维、合成纤维或纸；(2)第一涂覆步骤，即用涂覆溶液涂覆该基底的一面或两面，该涂覆溶液包含选自聚合物、碳化聚合物和石墨中的至少一种；和(3)通过热处理来对经涂覆的基底进行石墨化。
本申请提供一种石墨片，该石墨片包括内层和覆盖该内层一侧或两侧的石墨外层，该内层包含石墨纤维。
有益效果
本申请的石墨片由于在垂直方向上具有低热扩散率和在水平方向上具有高的热扩散率，因此具有高的水平/垂直方向热扩散率之比，且同时具有良好的柔韧性。
此外，可以使用相对便宜的纤维基底来代替价格昂贵的聚酰亚胺膜(PI膜)，以低制造成本制备石墨片。
附图说明
图1和图2是本申请实施例的石墨片的基底的表面和横截面的扫描电子显微镜(SEM)图像。
具体实施方式
本申请涉及一种石墨片，该石墨片通过热处理(i)包含天然纤维、合成纤维或纸的基底和(ii)设置在基底的一侧或两侧上的涂层而获得，涂层包括选自聚合物、碳化聚合物和石墨中的至少一种。
根据本申请的石墨片，基底可以由天然纤维构成，天然纤维主要分为纤维素纤维、蛋白纤维和矿物纤维。纤维素纤维可以包括(i)种子纤维，如棉花和木棉；(ii)茎纤维，如亚麻、苎麻、大麻和黄麻；(iii)水果纤维，如椰浆纤维，和(iv)叶片纤维，如马尼拉麻、蕉麻和剑麻。蛋白质纤维包括(i)羊纤维；(ii)丝纤维和(iii)毛发纤维。当本申请的石墨片的基底由天然纤维构成时，天然纤维优选为选自棉、麻、羊毛和丝绸中的至少一种。
此外，根据本申请的石墨片，基底可以由合成纤维构成，合成纤维主要分为有机纤维和无机纤维。有机纤维可以包括(i)再生纤维，包含纤维素基纤维(如人造丝(rayon)、天丝纤维(Tencel fiber)(或莱赛尔(lyocell))和莫代尔(modale))和蛋白质纤维；(ii)半合成纤维，包含纤维素基纤维(如醋酸纤维和三醋酸纤维)；或(iii)合成纤维，如聚酰胺纤维、聚酯纤维、聚氨酯纤维、聚乙烯纤维、聚氯乙烯纤维、聚氟乙烯纤维、聚乙烯醇纤维、丙烯酸纤维和聚丙烯纤维。当本申请的石墨片的基底由合成纤维构成时，合成纤维可以选自尼龙、聚酯、聚氨酯、聚乙烯、聚氯乙烯、聚氟乙烯、聚乙烯醇、丙烯酸和聚丙烯中的至少一种；或选自以下纤维素基纤维中的至少一种：人造丝、醋酸纤维和三醋酸纤维。
另外，根据本申请的石墨片，基底也可以由纸构成。
根据本申请的石墨片，涂层可以包含聚合物。聚合物可以选自聚酰亚胺、聚酰胺酸、聚氯乙烯、聚酯、聚氨酯、聚乙烯、聚氟乙烯、聚乙烯醇、丙烯酸和聚丙烯中的至少一种。特别地，聚合物可以选自重均分子量为200,000-300,000的聚酰亚胺、聚酰胺酸和聚氯乙烯中的至少一种。
根据本申请的石墨片，涂层可以包含碳化聚合物。碳化聚合物可以通过在惰性气体气氛(如氮气和氩气)中在800-1,800℃，特别是1,000-1,400℃的温度下对聚合物进行热处理而获得。碳化聚合物可以包含基于涂层总量的90％(重量)或90％(重量)以上的碳。根据所使用的聚合物的种类，碳化聚合物中所含的碳的量以聚合物的初始量为基准计为约2％-50％(重量)。
根据本申请的石墨片，涂层可以包含石墨。石墨可以是天然石墨或膨胀石墨。膨胀石墨是指用硫酸、硝酸等的混合物对天然石墨、热解石墨、凝析石墨等进行处理、洗涤、干燥，并在膨胀炉中在约1,000℃温度下对其进行膨胀而获得的石墨。
根据本申请的石墨片，涂层可以包括选自聚酰胺酸、聚酰亚胺和石墨中的至少一种。
本申请的石墨片在水平和垂直方向的热扩散率之比可以为300或300以上、400或400以上、500或500以上。具体而言，水平和垂直方向的热扩散率之比可以为300-2,000、300-1,800、300-1,500、400-1,250或500-1,000。
本申请的石墨片在水平方向的热扩散率可以为100-1,000mm2/s、200-800mm2/s或400-600mm2/s。
本申请的石墨片在垂直方向的热扩散率可以为2.0mm2/s或2.0mm2/s以下、1.0mm2/s或1.0mm2/s以下。具体来说，垂直方向的热扩散率可以为0.1-1mm2/s、0.2-2mm2/s或0.3-2mm2/s。
此外，根据MIT方法，在曲率半径(R)为5mm，折叠角为180度，负载为0.98N，折叠速度为90次/分钟的条件下测试时，本申请的石墨片在断裂之前的振动折叠次数为10,000或10,000以上。
本申请一实施方式中，石墨片的特征在于，基底的横截面形状与构成石墨片的天然纤维、合成纤维或纸的形状相同。例如，如图1所示，当基底由纤维素纤维构成时，石墨片的基底的横截面与纤维素纤维的形状相同。
本申请提供一种石墨片的制备方法，包括：(1)提供基底，该基底包含天然纤维、合成纤维或纸；(2)第一涂覆步骤，即用涂覆溶液涂覆该基底的一面或两面，该涂覆溶液包含选自聚合物、碳化聚合物和石墨中的至少一种；和(3)通过热处理来对经涂覆的基底进行石墨化。
在本方法的步骤(2)中，可以使用常规的涂覆方法，例如滚压法、棒涂法、浸涂法或喷涂法等。优选滚压法或棒涂法。特别地，当使用具有高粘度的液相聚酰胺酸作为涂覆溶液时，优选滚压法可有效地涂覆基底。
本申请一实施方式中，石墨片的制备方法还可进一步包括在第一涂覆步骤之后进行第二涂覆步骤，即将相同的涂覆溶液涂覆到第一涂层上。此处第一涂覆主要是为了用聚合物填充棉织物中的间隙，第二涂覆用于调节涂层厚度。优选地，可以进行1-3次第二涂覆步骤。
本申请另一实施方式中，石墨片的制备方法还可进一步包括在第一涂覆步骤之后对经涂覆的基底进行滚压。滚压使涂层的厚度均匀。
本申请又一实施方式中，涂覆溶液可以包含聚酰胺酸，并且该方法可以进一步包括在第一涂覆步骤之后对经涂覆的基底进行酰亚胺化。
本方法的步骤(3)可以包括碳化过程、石墨化过程和后处理过程。
在碳化过程中，可以通过在800-1,800℃，特别是1,000-1,400℃，更特别是约1,000℃下加热1-20小时来对基底和涂层进行碳化。
在石墨化过程中，可以通过在2,000-2,900℃，特别是约2,850℃下加热1-20小时来对经碳化的基底和涂层进行石墨化，以获得石墨片。
在后处理过程中，对在石墨化过程中获得的石墨片用酸或加压进行后处理以赋予石墨片柔韧性。
酸可以是任何可以插入石墨层间并且产生用于在石墨晶体的C轴方向上膨胀的酸离子(阴离子)的材料。优选硫酸。更优选浓度为95％(重量)或95％(重量)以上的浓硫酸溶液。例如，将石墨片浸渍在硫酸溶液中，如果需要，将其加热到典型的温度，使石墨层之间在C轴方向膨胀，从而得到柔性石墨片。
例如，可以使用辊压机施加压力。
此外，本申请提供一种石墨片，该石墨片包括包含石墨纤维的内层和覆盖该内层一侧或两侧的石墨外层。
内层可以由包括多个石墨纤维的纤维束构成。纤维束可以包括在多个石墨纤维之间形成的孔。内层可以包括织物，该织物中，由石墨纤维或石墨纤维束制成的纬纱和经纱被织造。
石墨外层包括覆盖内层一侧的第一石墨外层和覆盖内层另一侧的第二石墨外层。第一石墨外层和第二石墨外层可以部分地彼此连接。
实施例
以下通过实施例对本申请进行详细说明。以下实施例旨在进一步说明本申请而非限制其范围。
[实施例]
实施例1
(1)制备基底
准备平纹棉织物(100su，150mm×100mm，中国制造)作为由纤维素基纤维构成的基底。
(2)第一涂覆和第二涂覆
在25℃下通过滚压法将液相聚酰胺酸(制造商：KOLON PI，商品名：PAA Varnish，重均分子量：250,000)涂覆在基底的两面上，厚度为175μm。进行第二涂覆步骤，即将相同的涂覆溶液涂覆在第一涂层上，厚度为150μm，从而得到基底膜。
(3)酰亚胺化
将步骤(2)中制备的基底膜置于氮气气氛(约100托的压力)下，以1℃/分钟的速度升温。将基底膜在约400℃下加热约10小时，得到厚度为140-160μm的经酰亚胺化的基底膜。
(4)碳化、石墨化和后处理
将步骤(3)中制备的经酰亚胺化的基底膜置于氮气或惰性气体气氛(约100托的压力)下，以1℃/分钟的速度升温。将经酰亚胺化的基底膜在约1000℃下加热约3小时以进行碳化。然后以5℃/分钟的速度升温，经碳化的基底膜在约2,600℃下加热约1小时以进行石墨化。作为后处理，使用辊压机在10吨的负荷下压制经石墨化的基底片，得到厚度为约40μm的石墨片。
实施例2
按照与实施例1相同的方法制备厚度为约40μm的石墨片，不同的是使用人造丝织物代替棉织物。
对比例1
根据与实施例1相同的碳化、石墨化和后处理方法制备厚度为约40μm的石墨片，不同的是使用聚酰亚胺膜(厚度为约75μm，制造商：KOLON PI，商品名：PI Film 75μm)代替实施例1使用的棉织物作为基底膜。
实验例
<热扩散率的测定>
使用热扩散率测定装置(由Netsch公司制造，“LFA447Nanoflash”)根据光交流法测定实施例和对比例制备的石墨片在水平方向和垂直方向的热扩散率。特别地，将石墨片分别切割成Ф25.4mm和Ф12.6mm尺寸，在25℃下测定水平和垂直方向的热扩散率5次或5次以上，并计算其平均值。
<柔韧性测量>
通过MIT弹性试验评价实施例和对比例中制备的石墨片的柔韧性。在MIT弹性试验中，在曲率半径(R)为5mm，折叠角为180度，负载为0.98N，折叠速度为90次/分钟的条件下，将宽度为20mm的四边形试样进行重复折叠，直至断裂。通过MIT弹性试验中石墨片在断裂之前的振动折叠次数对其柔韧性进行评价。
结果如表1所示。
[表1]
根据如表1所示的测试结果，通过保持在水平方向上高的热扩散率和垂直方向上低的热扩散率，本申请的石墨片具有高的水平/垂直方向热扩散率之比。结果还证实了本申请的石墨片具有高的水平/垂直方向热扩散率之比且同时具有良好的柔韧性。由于本申请的石墨片使用棉或人造丝织物作为基底，因此可以以低成本进行生产，具有经济优势。
附图标记说明
102,106,110和112：石墨外层(涂层石墨)
104：石墨内层(基底层石墨)
114：包含石墨纤维的纤维束
116：用于扫描电子显微镜(SEM)图像的成型材料

Claims (17)

1.一种石墨片，所述石墨片在水平和垂直方向的热扩散率之比为300或300以上。
2.如权利要求1所述的石墨片，其特征在于，所述在水平和垂直方向的热扩散率之比为500或500以上。
3.如权利要求1所述的石墨片，其特征在于，根据MIT试验，在曲率半径为5mm，折叠角度为180度，负载为0.98N，折叠速度为90次/分钟的条件下进行测试时，所述石墨片在断裂之前的振动折叠次数为10,000或10,000以上。
4.一种石墨片，所述石墨片在垂直方向的热扩散率为2.0mm2/s或2.0mm2/s以下。
5.如权利要求4所述的石墨片，其特征在于，垂直方向的热扩散率为1.0mm2/s或1.0mm2/s以下。
6.一种石墨片的制备方法，所述方法包括：
(1)提供基底，所述基底包含天然纤维、合成纤维或纸；
(2)第一涂覆步骤，即用涂覆溶液涂覆所述基底的一面或两面，所述涂覆溶液包含选自聚合物、碳化聚合物和石墨中的至少一种；和
(3)通过热处理来对经涂覆的基底进行石墨化。
7.如权利要求6所述的石墨片的制备方法，进一步包括在所述第一涂覆步骤之后进行第二涂覆步骤，即将涂覆溶液涂覆到第一涂覆步骤后得到的涂层上。
8.如权利要求6所述的石墨片的制备方法，进一步包括在所述第一涂覆步骤之后对经涂覆的基底进行滚压。
9.如权利要求6所述的石墨片的制备方法，其特征在于，所述涂覆溶液包含聚酰胺酸，并且所述方法进一步包括在所述第一涂覆步骤之后对经涂覆的基底进行酰亚胺化。
10.如权利要求6所述的石墨片的制备方法，其特征在于，所述基底由选自棉、麻、羊毛和丝绸中的至少一种天然纤维构成。
11.如权利要求6所述的石墨片的制备方法，其特征在于，所述基底由选自人造丝、醋酸纤维和三醋酸纤维中的至少一种纤维素基纤维构成。
12.如权利要求6所述的石墨片的制备方法，其特征在于，所述基底由选自尼龙、聚酯、聚氨酯、聚乙烯、聚氯乙烯、聚氟乙烯、聚乙烯醇、丙烯酸和聚丙烯中的至少一种合成纤维构成。
13.一种石墨片，所述石墨片包括包含石墨纤维的内层和覆盖所述内层一侧或两侧的石墨外层。
14.如权利要求13所述的石墨片，其特征在于，所述内层由包括多个石墨纤维的纤维束构成。
15.如权利要求14所述的石墨片，其特征在于，所述纤维束包括在所述多个石墨纤维之间形成的孔。
16.如权利要求13所述的石墨片，其特征在于，所述石墨外层包括覆盖所述内层一侧的第一石墨外层和覆盖所述内层另一侧的第二石墨外层，且所述第一石墨外层和第二石墨外层部分地彼此连接。
17.如权利要求13所述的石墨片，其特征在于，所述内层包括织物，所述织物中，由石墨纤维或石墨纤维束构成的纬纱和经纱被织造。
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