CN113511895A - 一种TiC/石墨膜层状复合材料及其制备方法 - Google Patents

一种TiC/石墨膜层状复合材料及其制备方法 Download PDF

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CN113511895A
CN113511895A CN202110439008.8A CN202110439008A CN113511895A CN 113511895 A CN113511895 A CN 113511895A CN 202110439008 A CN202110439008 A CN 202110439008A CN 113511895 A CN113511895 A CN 113511895A
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张阔
于方丽
张海鸿
唐健江
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Abstract

本发明涉及无机非金属材料领域，公开了一种TiC/石墨膜层状复合材料及其制备方法，该复合材料按体积分数计，由23.2～84.9％的TiC陶瓷相和15.1～76.8％的石墨相组成，石墨和TiC在复合材料中逐层交替分布，并呈完美取向排列；其制备方法由Ti箔的预处理、Ti箔与石墨膜的逐层堆叠及后续的真空热压烧结三个步骤组成。本发明工艺简单，成本低廉，且制备出的材料微观结构均匀，致密度高。另外，本发明也适合WC、Cr2C3、MoC、ZrC等陶瓷与石墨膜复合材料的制备，因此大大扩展了碳化物陶瓷/石墨膜层状复合材料的制备方法。

Description

一种TiC/石墨膜层状复合材料及其制备方法
技术领域
本发明涉及功能材料及制备，特别涉及一种TiC/石墨膜层状复合材料及其制备方法。
背景技术
石墨膜具有耐高温、密度低、厚度可控、平面尺寸大、沿层方向热导率高、化学性能稳定等优点，其作为一种理想的热管理材料，已在计算机、手机等高产热量但又急需散热的电子设备中广泛应用。然而，石墨膜的强度非常低，极易破损，这一致命弱点使其应用受到一定限制。
为克服石墨膜强度低的弱点，一种有效的途径是将其与陶瓷、金属复合化制备出层状复合材料。特别地，相比于金属，陶瓷具有强度高、抗氧化性、耐蚀性、耐高温性、化学稳定性好等优点，将其与石墨复合后，不仅有望在部分领域取代金属/石墨膜层状复合材料，而且可在高温及一些特殊环境中(如低于400℃的富氧环境、腐蚀环境等)使用，因此可扩大热管理材料的应用范围。目前，陶瓷/石墨膜层状复合材料的制备工艺主要有：(1)陶瓷粘结剂与石墨膜的叠层热压烧结，如文献“多层石墨膜-陶瓷复合材料的制备及其导热性能”(材料热处理学报.2019,40,3:27-34)；(2)陶瓷先驱体在石墨膜预制体中的浸渍裂解，如“高热导率C/SiC复合材料的制备与性能研究”(硕士论文，2018)；(3)通过熔盐反应使石墨膜表面陶瓷化及随后的叠层热压烧结，如申请号为CN201910275350.1的中国专利“一种热管理用SiC/石墨膜层状复合材料及其制备方法”等。
然而，这些制备工艺均存在不足。例如，陶瓷粘结剂的制备不仅需要繁杂的料浆配置过程，而且粘结剂中有机物的的排出会产生气孔，从而使得制备出的材料致密度低，力学性能较差；通过熔盐反应使石墨膜表面陶瓷化的工艺虽然简单，但熔盐的挥发会造成设备污染，且成本较高、效率低；陶瓷先驱体在石墨膜预制体中的浸渍裂解不仅存在工艺复杂、周期较长、效率低等问题，而且裂解后产生的气体会污染环境。因此开发工艺简单、效率高、力学性能优异、环境友好的陶瓷/石墨膜层状复合材料制备技术具有非常重要的意义。
发明内容
本发明的目的在于，提供一种工艺简单、效率高、力学性能优异、环境友好的TiC/石墨膜层状复合材料及其制备方法。
为达到以上目的，本发明采用的制备方法为：
第一步，Ti箔的预处理；
第二步，将预处理后的Ti箔与石墨膜裁剪成直径相同的圆片，按“Ti箔圆片—石墨膜圆片—Ti箔圆片—石墨膜圆片……”的顺序逐层堆叠进石墨模具内；
第三步，将石墨模具放入真空热压烧结炉中，首先抽真空至0.01Pa以下，然后升温至1500℃，并在30MPa压力下保温10小时，随后在烧结温度为1800～2000℃、烧结压力为30～50MPa、保温时间为1～3h的进行真空热压烧结，冷却后得到TiC/石墨膜层状复合材料。
所述第一步中Ti箔的厚度≤50微米。
所述第一步Ti箔的预处理，包括下述步骤：
(1)将Ti箔浸入到丙酮溶液并超声振荡进行表面除油；
(2)将表面除油后的Ti箔浸入到酸液中超声振荡进行酸洗，除去Ti箔表面的氧化层；
(3)用蒸馏水将酸洗后的Ti箔清洗干净，在真空烘箱中干燥后，得预处理的Ti箔。
所述酸液含体积浓度6％的硝酸、30％的盐酸及0.5％的氢氟酸。
所述第二步中石墨膜的厚度大于等于Ti箔，小于等于100微米。
所述第二步中石墨模具的内壁涂覆有BN。
按以上制备方法制成的TiC/石墨膜层状复合材料，其特征在于，按体积分数计，由23.2～84.9％的TiC陶瓷相和15.1～76.8％的石墨相组成块体，其中石墨和TiC在复合材料中逐层交替分布，并呈完美取向排列。
与现有技术相比，本发明具有如下优点：
本发明利用Ti与石墨的反应，在真空热压烧结过程中将Ti箔直接转变为TiC层，从而制备出TiC/石墨膜层状复合材料，由于不需要繁杂的浆料配制过程、石墨膜表面的预陶瓷化处理或较长周期的先驱体浸渍裂解工艺，因此制备工艺简单、效率高、成本低。另外，通过控制Ti箔或石墨膜的厚度，可方便对复合材料中TiC及石墨膜的体积分数进行调控。
本发明所制备的复合材料由交替分布且互相平行的TiC层和石墨层组成，且两者之间的界面结合良好。其制备方法由①Ti箔的预处理、②Ti箔与石墨膜的逐层堆叠及③TiC/石墨膜层状复合材料的真空热压烧结三个步骤组成。本发明制备工艺简单，成本低廉，且制备出的材料微观结构均匀，致密度高，性能优异。另外，本发明也适合WC、Cr2C3、MoC、ZrC等陶瓷与石墨膜层状复合材料的制备，因此大大扩展了碳化物陶瓷/石墨膜层状复合材料的制备方法。
附图说明
图1是本发明实施例1的TiC/石墨膜层状复合材料显微形貌照片。
具体实施方式
以下通过附图及表格(具体实施例)对本发明作进一步的详细说明。
一种TiC/石墨膜层状复合材料，按体积分数计，由表1所示的TiC和石墨膜组成块体，本发明TiC/石墨膜层状复合材料的制备方法，包括下述步骤：
第一步，对Ti箔进行预处理，具体步骤如下：
(1)将表1中不同厚度的Ti箔浸入到丙酮溶液并超声振荡30分钟，进行表面除油；
(2)将表面除油后的Ti箔浸入到含体积浓度为6％硝酸、30％盐酸及0.5％氢氟酸的酸液中超声振荡10分钟，进行酸洗，除去Ti箔表面的氧化层；
(3)用蒸馏水将酸洗后的Ti箔清洗干净，在真空烘箱中干燥后，得预处理的Ti箔。
第二步，将预处理后的Ti箔与表1中不同厚度的石墨膜裁剪成直径相同的圆片，按“Ti箔圆片—石墨膜圆片—Ti箔圆片—石墨膜圆片……”的顺序逐层堆叠进内壁涂覆BN的石墨模具内；
第三步，将石墨模具放入真空热压烧结炉中，首先抽真空至0.01Pa以下，然后升温至1500℃，在30MPa压力下保温10小时，随后按表1所示的条件进行真空热压烧结，冷却后得到TiC/石墨膜层状复合材料。
表1复合材料组成及烧结工艺参数
Figure BDA0003034281130000041
由图1可以看出，石墨膜和TiC在复合材料中逐层交替分布，并呈完美取向排列。且两者之间的界面结合良好。

Claims (7)

1.一种TiC/石墨膜层状复合材料的制备方法，其特征在于，包括下述步骤：
第一步，Ti箔的预处理；
第二步，将预处理后的Ti箔与石墨膜裁剪成直径相同的圆片，按“Ti箔圆片—石墨膜圆片—Ti箔圆片—石墨膜圆片……”的顺序逐层堆叠进石墨模具内；
第三步，将石墨模具放入真空热压烧结炉中，首先抽真空至0.01Pa以下，然后升温至1500℃，并在30MPa压力下保温10小时，随后在烧结温度为1800～2000℃、烧结压力为30～50MPa、保温时间为1～3h的进行真空热压烧结，冷却后得到TiC/石墨膜层状复合材料。
2.如权利要求1所述的一种TiC/石墨膜层状复合材料的制备方法，其特征在于，所述第一步中Ti箔的厚度≤50微米。
3.如权利要求1或2所述的一种TiC/石墨膜层状复合材料的制备方法，其特征在于，所述第一步Ti箔的预处理，包括下述步骤：
(1)将Ti箔浸入到丙酮溶液并超声振荡进行表面除油；
(2)将表面除油后的Ti箔浸入到酸液中超声振荡进行酸洗，除去Ti箔表面的氧化层；
(3)用蒸馏水将酸洗后的Ti箔清洗干净，在真空烘箱中干燥后，得预处理的Ti箔。
4.如权利要求3所述的一种TiC/石墨膜层状复合材料的制备方法，其特征在于，所述酸液含体积浓度6％的硝酸、30％的盐酸及0.5％的氢氟酸。
5.如权利要求1所述的一种TiC/石墨膜层状复合材料的制备方法，其特征在于，所述第二步中石墨膜的厚度大于等于Ti箔，小于等于100微米。
6.如权利要求1所述的一种TiC/石墨膜层状复合材料的制备方法，其特征在于，所述第二步中石墨模具的内壁涂覆有BN。
7.一种如权利要求1所述的制备方法制成的TiC/石墨膜层状复合材料，其特征在于，按体积分数计，由23.2～84.9％的TiC陶瓷相和15.1～76.8％的石墨相组成块体，其中石墨和TiC在复合材料中逐层交替分布，并呈完美取向排列。
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CN114055864A (zh) * 2021-11-05 2022-02-18 河北宇天材料科技有限公司 一种复合结构导热板及其制备方法和应用

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