CN104812204A - 用于石墨散热片的制造工艺 - Google Patents

用于石墨散热片的制造工艺 Download PDF

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CN104812204A
CN104812204A CN201410036320.2A CN201410036320A CN104812204A CN 104812204 A CN104812204 A CN 104812204A CN 201410036320 A CN201410036320 A CN 201410036320A CN 104812204 A CN104812204 A CN 104812204A
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CN104812204B (zh
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金闯
杨晓明
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Sidike New Materials Jiangsu Co Ltd
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Priority to CN201710665173.9A priority patent/CN107573072A/zh
Priority to CN201410036320.2A priority patent/CN104812204B/zh
Priority to CN201710665185.1A priority patent/CN108206164A/zh
Priority to CN201710095581.5A priority patent/CN107043258A/zh
Priority to CN201710095543.XA priority patent/CN107043108B/zh
Priority to CN201710095545.9A priority patent/CN107043257A/zh
Priority to CN201710665192.1A priority patent/CN108646885A/zh
Priority to CN201710095575.XA priority patent/CN107043255A/zh
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Abstract

本发明一种用于石墨散热片的制造工艺，包括：在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成；石墨改性剂由以下重量份的组分组成：二苯甲酮四酸二酐20~25份，均苯四甲酸二酐12~18份，二氨基二苯甲烷20~28份，二甲基甲酰胺20~25份，N-甲基吡咯烷酮8~10份，乙二醇1.5~2.5份，聚二甲基硅氧烷2~3份，邻苯二甲酸二丁酯0.8~1.5份；将处理后的聚酰亚胺薄膜从室温升至1200℃后获得预烧制的碳化膜；将碳化膜升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜。本发明实现了导热性能的均匀性的同时，提高了产品的散热性能稳定性、可靠性，大大降低了产品的成本。

Description

用于石墨散热片的制造工艺
技术领域
本发明涉及一种用于石墨散热片的制造工艺，属于石墨片技术领域。
背景技术
随着现代微电子技术高速发展，电子设备（如笔记本电脑、手机、平板电脑等）日益变得超薄、轻便，这种结构使得电子设备内部功率密度明显提高，运行中所产生的热量不易排出、易于迅速积累而形成高温。另一方面，高温会降低电子设备的性能、可靠性和使用寿命。因此，当前电子行业对于作为热控系统核心部件的散热材料提出越来越高的要求，迫切需要一种高效导热、轻便的材料迅速将热量传递出去，保障电子设备正常运行。
现有技术中聚酰亚胺薄膜大多用于柔性电路板，虽然有采用聚酰亚胺薄膜烧结获得石墨散热片，从而贴覆在热源上，但是受限于聚酰亚胺薄膜的产品质量和性能的良莠不齐，影响到了散热双面贴膜散热性能的发挥，存在以下技术问题：散热不均匀，易出现胶带局部过热，提高了产品的散热性能不稳定、可靠性性能差，不利于产品质量管控，影响产品的竞争力。
发明内容
本发明发明目的是提供一种用于石墨散热片的制造工艺，该制造工艺获得的用于石墨散热片在垂直方向和水平方向均提高了导热性能，避免局部过热，实现了导热性能的均匀性的同时，提高了产品的散热性能稳定性、可靠性，大大降低了产品的成本。
为达到上述发明目的，本发明采用的技术方案是：一种用于石墨散热片的制造工艺，其特征在于：所述石墨散热片通过以下步骤获得：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成；
所述石墨改性剂由以下重量份的组分组成：
二苯甲酮四酸二酐               20~25份，    
均苯四甲酸二酐                 12~18份，
二氨基二苯甲烷                 20~28份，
二甲基甲酰胺                   20~25份，
N-甲基吡咯烷酮                 8~10份，    
乙二醇                         1.5~2.5份，    
聚二甲基硅氧烷                 2~3份，
邻苯二甲酸二丁酯               0.8~1.5份；
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
上述技术方案中进一步改进的方案如下：
1、上述技术方案中，所述石墨改性剂的粘度为30000~48000CP。
2、上述技术方案中，包括以下步骤：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成，所述石墨改性剂的粘度为30000~48000CP；
所述石墨改性剂由以下重量份的组分组成：
二苯甲酮四酸二酐               20~25份，    
均苯四甲酸二酐                 12~18份，
二氨基二苯甲烷                 20~28份，
二甲基甲酰胺                   20~25份，
N-甲基吡咯烷酮                 8~10份，    
乙二醇                         1.5~2.5份，    
聚二甲基硅氧烷                 2~3份，
邻苯二甲酸二丁酯               0.8~1.5份；
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
由于上述技术方案运用，本发明与现有技术相比具有下列优点和效果：
1、本发明用于石墨散热片的制造工艺，其结构中石墨层由上、下表面均涂覆一层石墨改性剂的聚酰亚胺薄膜制备而成，提高了在垂直方向和水平方向的导热性能，避免胶带局部过热，实现了胶带导热性能的均匀性；其次，其位于聚酰亚胺薄膜表面的石墨改性剂由二苯甲酮四酸二酐20~25份、均苯四甲酸二酐12~18份、二氨基二苯甲烷20 ~28份、二甲基甲酰胺30~35份、乙二醇1.5~2.5份、聚二甲基硅氧烷2~3份组成，涂覆于聚酰亚胺薄膜上，填充了加热过程中的针孔，提高了结晶度同时，也克服了热收缩过大导致的不均匀，提高了石墨层双向拉伸性能。
2、本发明用于石墨散热片的制造工艺，其位于聚酰亚胺薄膜表面的石墨改性剂由二苯甲酮四酸二酐20~25份、均苯四甲酸二酐12~18份、二氨基二苯甲烷20 ~28份、二甲基甲酰胺20~25份、N-甲基吡咯烷酮8~10份、乙二醇1.5~2.5份、聚二甲基硅氧烷2~3份组成，采用二甲基甲酰胺20~25份、N-甲基吡咯烷酮8~10份降低了共沸点并且平滑的沸点区，改善了最终产品成膜的平坦性和柔韧性；；其次，二甲基甲酰胺20~25份、N-甲基吡咯烷酮8~10份和邻苯二甲酸二丁酯0.8~1.5 份聚酰亚胺薄膜表面，防止气泡产生，更有利于填充聚酰亚胺薄膜的微小针孔，改善了散热贴片导热性能的均匀性。
3、本发明用于石墨散热片的制造工艺，在预烧制的碳化膜和石墨化之间增加压延步骤，以及再形成导热石墨贴片后再次压延，避免了褶皱和石墨化烧结过程中的体积收缩，提高了致密性和结晶度，进一步提高了在垂直方向和水平方向的导热性能。
具体实施方式
下面结合实施例对本发明作进一步描述：
实施例：一种用于石墨散热片的制造工艺，所述石墨散热片通过以下步骤获得：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成；
所述石墨改性剂由以下重量份的组分组成：
表1
  实施例1 实施例2 实施例3 实施例4 实施例5
二苯甲酮四酸二酐 20 22 23.5 24 25
均苯四甲酸二酐 12 15 13.5 18 16.5
二氨基二苯甲烷 28 20 26 25 23.5
二甲基甲酰胺 25 21 22.5 24 22
N-甲基吡咯烷酮 8 8.5 10 9.5 9
乙二醇 2.5 2.2 1.5 1.8 2
聚二甲基硅氧烷 3 2.4 2.8 2 2.5
邻苯二甲酸二丁酯 1.4 0.8 1.2 1 1.5
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
上述石墨改性剂的粘度为30000~48000CP。
一种上述石墨散热片的制造工艺，包括以下步骤：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成，所述石墨改性剂的粘度为30000~48000CP；
所述石墨改性剂由以下重量份的组分组成：
表2
  实施例1 实施例2 实施例3 实施例4 实施例5
二苯甲酮四酸二酐 20 22 23.5 24 25
均苯四甲酸二酐 12 15 13.5 18 16.5
二氨基二苯甲烷 28 20 26 25 23.5
二甲基甲酰胺 25 21 22.5 24 22
N-甲基吡咯烷酮 8 8.5 10 9.5 9
乙二醇 2.5 2.2 1.5 1.8 2
聚二甲基硅氧烷 3 2.4 2.8 2 2.5
邻苯二甲酸二丁酯 1.4 0.8 1.2 1 1.5
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
采用上述制造工艺时，获得用于石墨散热片其结构中石墨层由上、下表面均涂覆一层石墨改性剂的聚酰亚胺薄膜制备而成，提高了在垂直方向和水平方向的导热性能，避免胶带局部过热，实现了胶带导热性能的均匀性；其次，其位于聚酰亚胺薄膜表面的石墨改性剂由二苯甲酮四酸二酐20~25份、均苯四甲酸二酐12~18份、二氨基二苯甲烷20 ~28份、二甲基甲酰胺30~35份、乙二醇1.5~2.5份、聚二甲基硅氧烷2~3份组成，涂覆于聚酰亚胺薄膜上，填充了加热过程中的针孔，提高了结晶度同时，也克服了热收缩过大导致的不均匀，提高了石墨层双向拉伸性能，也降低了共沸点并且平滑的沸点区，改善了最终产品成膜的平坦性和柔韧性；再次，聚酰亚胺薄膜表面具有石墨改性剂，改善了双面贴膜中石墨层与导热胶粘层导热性能，且采用压延机压延所述预烧制的碳化膜，避免了褶皱和石墨化烧结过程中的体积收缩，提高了致密性和结晶度，进一步提高了在垂直方向和水平方向的导热性能。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (3)

1. 一种用于石墨散热片的制造工艺，其特征在于：所述石墨散热片通过以下步骤获得：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成；
所述石墨改性剂由以下重量份的组分组成：
二苯甲酮四酸二酐               20~25份，    
均苯四甲酸二酐                 12~18份，
二氨基二苯甲烷                 20~28份，
二甲基甲酰胺                   20~25份，
N-甲基吡咯烷酮                 8~10份，    
乙二醇                         1.5~2.5份，    
聚二甲基硅氧烷                 2~3份，
邻苯二甲酸二丁酯               0.8~1.5份；
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
2. 根据权利要求1所述的用于石墨散热片的制造工艺，其特征在于：所述石墨改性剂的粘度为30000~48000CP。
3. 一种根据权利要求1或2所述的用于石墨散热片的制造工艺，其特征在于：包括以下步骤：
步骤一、在聚酰亚胺薄膜的上、下表面分别涂覆石墨改性剂获得处理后的聚酰亚胺薄膜，处理后的聚酰亚胺薄膜由聚酰亚胺薄膜、第一涂覆层和第二涂覆层组成，所述石墨改性剂的粘度为30000~48000CP；
所述石墨改性剂由以下重量份的组分组成：
二苯甲酮四酸二酐               20~25份，    
均苯四甲酸二酐                 12~18份，
二氨基二苯甲烷                 20~28份，
二甲基甲酰胺                   20~25份，
N-甲基吡咯烷酮                 8~10份，    
乙二醇                         1.5~2.5份，    
聚二甲基硅氧烷                 2~3份，
邻苯二甲酸二丁酯               0.8~1.5份；
步骤二、将处理后的聚酰亚胺薄膜在惰性气体保护下，从室温升至240℃~260℃，保温后升至480℃~500℃，保温后再升温至780℃~820℃，保温后升至1200℃后冷却，从而获得预烧制的碳化膜；
步骤三、将碳化膜升温至2350℃~2450℃，保温，再升温至2850℃~2950℃后冷却，从而获得主烧制的石墨膜；
步骤四、然后将步骤三所得的主烧制的石墨膜进行压延从而获得所述导热石墨贴片。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551392A (zh) * 2017-08-29 2018-01-09 成都三乙医疗科技有限公司 一种用于热疗的热导电片
WO2022198661A1 (zh) * 2021-03-26 2022-09-29 浙江华熔科技有限公司 一种超薄导热石墨膜及其制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114714687B (zh) * 2022-03-30 2023-09-29 安徽碳华新材料科技有限公司 一种不含卤素残留的石墨散热膜的制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1661856A1 (en) * 2003-09-02 2006-05-31 Kaneka Corporation Filmy graphite and process for producing the same
WO2008149920A1 (ja) * 2007-06-07 2008-12-11 Kaneka Corporation グラファイト複合フィルム
CN102555389A (zh) * 2010-12-15 2012-07-11 财团法人工业技术研究院 聚酰亚胺薄膜层合物及包含其的金属层压板
CN102757736A (zh) * 2011-04-29 2012-10-31 苏州沛德导热材料有限公司 一种石墨导热胶带及其生产工艺
CN103043657A (zh) * 2012-12-28 2013-04-17 苏州斯迪克新材料科技股份有限公司 胶带用石墨散热片
CN103059761A (zh) * 2012-12-28 2013-04-24 斯迪克新型材料（江苏）有限公司 高导热系数的石墨散热胶带

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9814835D0 (en) * 1998-07-08 1998-09-09 Europ Org For Nuclear Research A thermal management board
JP2005119887A (ja) * 2003-10-14 2005-05-12 Matsushita Electric Ind Co Ltd 高熱伝導性部材及びその製造方法、並びにそれを用いた放熱システム
JP5069860B2 (ja) * 2006-01-31 2012-11-07 株式会社カネカ グラファイトフィルム
CN101687647B (zh) * 2007-05-17 2013-04-17 株式会社钟化 石墨膜及石墨复合膜
JP2010003981A (ja) * 2008-06-23 2010-01-07 Kaneka Corp 厚み方向にグラファイトが配向した熱伝導シート
US20120141758A1 (en) * 2010-12-07 2012-06-07 E.I. Du Pont De Nemours And Company Filled polyimide films and coverlays comprising such films
JP5450891B2 (ja) * 2011-03-28 2014-03-26 株式会社カネカ グラファイトフィルムの製造方法
EP2612879A4 (en) * 2011-07-08 2015-04-01 Mitsui Chemicals Inc POLYIMIDE RESIN COMPOSITION AND LAMINATE THEREWITH
CN102560453B (zh) * 2012-03-08 2013-12-11 哈尔滨工业大学 利用石墨烯增强聚酰亚胺树脂碳化制备碳化膜的方法
TWM446318U (zh) * 2012-08-09 2013-02-01 Hugetemp Energy Ltd 柔性石墨紙之材料的堆疊結構
CN103045119B (zh) * 2012-12-28 2014-04-23 苏州斯迪克新材料科技股份有限公司 超高导热系数散热双面胶带

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1661856A1 (en) * 2003-09-02 2006-05-31 Kaneka Corporation Filmy graphite and process for producing the same
WO2008149920A1 (ja) * 2007-06-07 2008-12-11 Kaneka Corporation グラファイト複合フィルム
CN102555389A (zh) * 2010-12-15 2012-07-11 财团法人工业技术研究院 聚酰亚胺薄膜层合物及包含其的金属层压板
CN102757736A (zh) * 2011-04-29 2012-10-31 苏州沛德导热材料有限公司 一种石墨导热胶带及其生产工艺
CN103043657A (zh) * 2012-12-28 2013-04-17 苏州斯迪克新材料科技股份有限公司 胶带用石墨散热片
CN103059761A (zh) * 2012-12-28 2013-04-24 斯迪克新型材料（江苏）有限公司 高导热系数的石墨散热胶带

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551392A (zh) * 2017-08-29 2018-01-09 成都三乙医疗科技有限公司 一种用于热疗的热导电片
WO2022198661A1 (zh) * 2021-03-26 2022-09-29 浙江华熔科技有限公司 一种超薄导热石墨膜及其制备方法

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