CN112552066A - 一种2d碳/碳pecvd载板的制备方法 - Google Patents
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Abstract
本发明公开一种2D碳/碳PECVD载板的制备方法,其是一种新的PECVD载板产品工艺,使载板产品在使用过程中不仅保持板材的整体性能及使用性能,同时在工艺方面具有低生产成本,易批量生产的特点,生产的载板产品层间结合强度高、碳纤维含量高、平整性好、使用寿命长等特点,大大增强了PECVD载板产品的刚度,有效改善板材使用变形、分层及断裂的问题,且生产成本低。
Description
技术领域
本发明涉及一种2D碳/碳PECVD载板的制备方法。
背景技术
2D碳/碳PECVD载板是硅片镀膜设备的主要消耗部件之一,其工作原理为将需要镀膜的硅片平整的放置在PECVD载板的工位上,经传送带运输到PECVD镀膜设备中的等离子腔室,然后在一定工艺条件下进行PECVD镀膜。随着太阳能光伏行业的迅速发展,市场对硅片镀膜的质量和产量和产能需求均不断提高,2D碳碳板材使用环境也愈加恶劣,对现有的碳碳载板性能提出更高的要求。当前技术环境下,应用广泛的载板结构有三维针刺结构以及二维叠层结构(即2D板材)。两者各具特色,针刺结构盖板整体性好,不易变形,但在使用过程中容易发生断裂;而二维叠层结构盖板强度高,无断裂问题,但存在变形及层间分层问题。
为适应PECVD镀膜设备对载板的需要,国内PECVD载板产品无论从产品性能,还是结构设计上都不断进行改进。中国专利CN 106364023 A一种碳/碳平板及其制备方法,采用的是碳布加短纤维黏合剂的方式进行热压成型,然后通过气相沉积致密至符合使用密度要求的碳/碳板材。该方法是采用增加层间组分提高层间结合力的方法,提高二维板材的整体性能。但这种板材的主要通过气相CVD工艺增密,故其制备周期长、成本高、性价比低,同时这种结构的载板使用过程中存在断裂的风险。
发明内容
为解决以上现有技术存在的问题,本发明提出一种2D碳/碳PECVD载板的制备方法。
本发明可通过以下技术方案予以解决:
一种2D碳/碳PECVD载板的制备方法,包括如下步骤:
1)将T700级12k碳纤维编织成平纹碳布;
2)对所述12K平纹碳布进行高温活化处理;
3)将所述高温处理过的平纹碳布制备成酚醛树脂预浸料;
4)通过挤压的方法将所述酚醛树脂预浸料丝束展宽;
5)所述酚醛树脂预浸料铺层后经热压固化成型得到树脂基模压板;
6)碳化处理;
7)树脂浸渍-碳化工艺增密,包括真空浸渍-压力浸渍-压力固化-碳化工艺增密;
8)石墨化处理制得2D碳/碳复合材料板材;
9)将所述2D碳/碳复合材料板材进行表面热解炭涂层处理;
10)机加工。
进一步地,所述步骤1)中所述平纹碳布面密度为360~450g/m2。
进一步地,所述步骤2中,高温活化处理温度为1500~2000℃,保温2~4h。
进一步地,所述步骤3)中所述酚醛树脂预浸料,其树脂含量为40%~44%,挥发分含量小于8%;
进一步地,所述步骤4)中,所述丝束宽度4mm~4.5mm。
进一步地,所述步骤5)中,固化温度150~180℃,压力2~4MPa;预浸料铺层根据板材厚度设计,即厚度d=L*S/h,其中L为碳布铺层层数,S为碳布面密度,h为板材所设计的纤维体积密度。
进一步地,所述步骤6)中,碳化温度在700~900℃之间,保温2~4h;且碳化处理时,为保证板材的平整性,板材上面施加压力,压力不小于0.15MPa。
进一步地,所述步骤7)中,所述浸渍压力与固化压力不低于1.5MPa。
进一步地,所述步骤8)中,所述石墨化处理温度在2000~2400℃,保温时间1~4h。
进一步地,所述步骤9)包括:将所述2D碳/碳复合材料板材放入化学气相沉积炉中,沉积温度为1000~1200℃,通入天然气或丙烷或其它碳氢化合物,以氩气为稀释气体,控制炉压为500~4000Pa,进行10~30h表面热解碳涂层处理。
有益效果
与现有技术相比,通过本发明制备的2D碳/碳PECVD载板具有板材层间结合强度高、碳纤维含量高、平整性好、使用寿命长等特点,产品的刚度高,有效改善了2D碳/碳板材使用变形的问题,同时生产成本低。
附图说明
图1为本发明工艺路线图
具体实施方式
以下通过特定的具体实施例说明本发明的实施方式,本领域的技术人员可由本说明书所揭示的内容轻易地了解本发明的其他优点及功效。
实施例1
一种2D碳/碳PECVD载板的制备方法(如图1所示),包括如下步骤:
(1)将T700级12k碳纤维编织成平纹碳布,平纹碳布面密度为360g/m2;
(2)对12K平纹碳布进行高温活化处理以提高碳纤维的表面活性,高温预处理温度为1500℃,保温2h;
(3)将高温处理过的平纹碳布制备成酚醛树脂预浸料,其树脂含量为40%,挥发分含量7%,酚醛树脂为钡酚醛树脂、氨酚醛树脂、硼酚醛树脂中的一种或多种,本实施例中,酚醛树脂为硼酚醛树脂;
(4)通过挤压的方法将预浸平纹碳布丝束展宽,丝束宽度4mmmm;
(5)预浸碳布铺层后经热压固化成型得到树脂基模压板,其中固化温度150℃,压力2MPa;预浸料铺层根据板材厚度设计,即厚度d=L*S/h,(其中L为碳布铺层层数,S为碳布面密度,h为板材所设计的纤维体积密度);
(6)碳化处理,碳化温度在700℃之间,保温2h;且碳化处理时,板材上面施加压力以保证2D碳/碳复合材料板材碳化后具有较高的平整度,压力0.15MPa;
(7)树脂浸渍-碳化工艺增密,真空浸渍-压力浸渍-压力固化-碳化工艺增密,其中浸渍压力与固化压力1.5MPa;
(8)石墨化处理,石墨化处理温度在2000℃,保温时间1h;
(9)表面热解炭涂层处理,2D碳/碳复合材料板材放入化学气相沉积炉中,沉积温度为100℃,通入丙烷,以氩气为稀释气体,控制炉压为500Pa,进行10h表面热解碳涂层处理;
(10)机加工。
经过上述步骤,得到纤维含量高、平整性好、层间强度高、使用寿命长的高性能PECVD载板。
实施例2
一种2D碳/碳PECVD载板的制备方法,包括如下步骤:
(1)将T700级12k碳纤维编织成平纹碳布,平纹碳布面密度为450g/m2;
(2)对12K平纹碳布进行高温活化处理以提高碳纤维的表面活性,高温预处理温度为2000℃,保温4h;
(3)将高温处理过的平纹碳布制备成酚醛树脂预浸料,其树脂含量为44%,挥发分含量6%,酚醛树脂为钡酚醛树脂、氨酚醛树脂、硼酚醛树脂中的一种或多种,本实施例中,酚醛树脂为氨酚醛树脂;
(4)通过挤压的方法将预浸平纹碳布丝束展宽,丝束宽度4.5mm;
(5)预浸碳布铺层后经热压固化成型得到树脂基模压板,其中固化温度180℃,压力4MPa;预浸料铺层根据板材厚度设计,即厚度d=L*S/h,(其中L为碳布铺层层数,S为碳布面密度,h为板材所设计的纤维体积密度);
(6)碳化处理,碳化温度在900℃之间,保温4h;且碳化处理时,板材上面施加压力以保证2D碳/碳复合材料板材碳化后具有较高的平整度,压力0.2MPa;
(7)树脂浸渍-碳化工艺增密,真空浸渍-压力浸渍-压力固化-碳化工艺增密,其中浸渍压力与固化压力1.6MPa;
(8)石墨化处理,石墨化处理温度在2400℃,保温时间4h;
(9)表面热解炭涂层处理,2D碳/碳复合材料板材放入化学气相沉积炉中,沉积温度为1200℃,通入天然气,以氩气为稀释气体,控制炉压为4000Pa,进行30h表面热解碳涂层处理;
(10)机加工。
经过上述步骤,得到纤维含量高、平整性好、层间强度高、使用寿命长的高性能PECVD载板。
实施例3
一种2D碳/碳PECVD载板的制备方法,包括如下步骤:
(1)双向碳布编织,所述双向碳布采用12k碳纤维丝束编织,碳布面密度为400g/m2;
(2)高温预处理双向碳布以提高碳纤维的表面活性,高温热处理温度为1500℃,保温2h;
(3)将热处理后的双向碳布制成酚醛树脂预浸料,其中酚醛树脂含量为42%,挥发分含量为6%,酚醛树脂为钡酚醛树脂、氨酚醛树脂、硼酚醛树脂中的一种或多种,本实施例中,酚醛树脂为钡酚醛树脂。
(4)通过滚轴压挤的方法将预浸碳布丝束展宽,丝束宽度4.4mm;
(5)预酚醛浸碳布铺层并经热压固化得到树脂基模压板,其中固化温度180℃,压力2.5MPa,酚醛预浸料铺层根据板材厚度设计,即厚度d=L*S/h,(其中L为双向碳布铺层层数,S为双向碳布面密度,h为板材所设计的纤维体积密度);
(6)碳化处理,碳化温度在760℃,保温2h;碳化过程中,树脂基板材上面施加压力以保证其碳化后具有较高的平整度,压力0.17MPa;
(7)树脂浸渍/碳化工艺增密,其中固化压力3MPa;
(8)高温处理,高温处理温度为2000℃,保温时间4h;
(9)热解炭表面涂层,2D碳/碳板材放入CVD炉中,沉积温度为1100℃,通入天然气、丙烷等碳氢化合物,以氩气为稀释气体,控制炉压为2000Pa,进行30h热解碳涂层处理;
(10)机械加工。
经过上述步骤,得到纤维含量高、平整性好、层间强度高、使用寿命长的高性能PECVD载板。
实施例4
一种2D碳/碳PECVD载板的制备方法,包括如下步骤:
(1)双向碳布编织,所述双向碳布采用12k碳纤维丝束编织,碳布面密度为450g/m2;
(2)高温预处理双向碳布以提高碳纤维的表面活性,高温预处理温度为1700℃,保温4h;
(3)将热处理后的双向碳布制成酚醛树脂预浸料,其中酚醛树脂含量为44%,挥发分含量为5%,酚醛树脂为钡酚醛树脂、氨酚醛树脂、硼酚醛树脂中的一种或多种,本实施例中,酚醛树脂为氨酚醛树脂;
(4)通过滚轴压挤的方法将预浸碳布丝束展宽,丝束宽度4mm;
(5)预酚醛浸碳布铺层并经热压固化得到树脂基模压板,其中固化温度170℃,压力2.0MPa,酚醛预浸料铺层根据板材厚度设计,即厚度d=L*S/h,(其中L为双向碳布铺层层数,S为双向碳布面密度,h为板材所设计的纤维体积密度);
(6)碳化处理,碳化温度在850℃之间,保温2h;碳化过程中,树脂基板材上面施加压力以保证其碳化后具有较高的平整度,压力0.3MPa;
(7)树脂浸渍/碳化工艺增密,其中固化压力2MPa;
(8)高温处理,高温处理温度为2200℃,保温时间4h;
(9)热解炭表面涂层,2D碳/碳板材放入CVD炉中,沉积温度为1100℃,通入天然气、丙烷等碳氢化合物,以氩气为稀释气体,控制炉压为3000Pa,进行30h热解碳涂层处理;
(10)机械加工。
经过上述步骤,得到纤维含量高、平整性好、层间强度高、使用寿命长的高性能PECVD载板。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种2D碳/碳PECVD载板的制备方法,包括如下步骤:
1)将T700级12k碳纤维编织成平纹碳布;
2)对所述12K平纹碳布进行高温活化处理;
3)将所述高温处理过的平纹碳布制备成酚醛树脂预浸料;
4)通过挤压的方法将所述酚醛树脂预浸料丝束展宽;
5)所述酚醛树脂预浸料铺层后经热压固化成型得到树脂基模压板;
6)碳化处理;
7)树脂浸渍-碳化工艺增密,包括真空浸渍-压力浸渍-压力固化-碳化工艺增密;
8)石墨化处理制得2D碳/碳复合材料板材;
9)将所述2D碳/碳复合材料板材进行表面热解炭涂层处理;
10)机加工。
2.根据权利要求1所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤1)中所述平纹碳布面密度为360~450g/m2。
3.根据权利要求2所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤2中,高温活化处理温度为1500~2000℃,保温2~4h。
4.根据权利要求3所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤3)中所述酚醛树脂预浸料,其树脂含量为40%~44%,挥发分含量小于8%。
5.根据权利要求4所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤4)中,所述丝束宽度4mm~4.5mm。
6.根据权利要求5所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤5)中,固化温度150~180℃,压力2~4MPa;预浸料铺层根据板材厚度设计,即厚度d=L*S/h,其中L为平纹碳布铺层层数,S为平纹碳布面密度,h为板材所设计的纤维体积密度。
7.根据权利要求6所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤6)中,碳化温度在700~900℃之间,保温2~4h;且碳化处理时,板材上面施加压力,压力不小于0.15MPa。
8.根据权利要求7所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤7)中,所述浸渍压力与固化压力不低于1.5MPa。
9.根据权利要求8所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤8)中,所述石墨化处理温度在2000~2400℃,保温时间1~4h。
10.根据权利要求9所述的一种2D碳/碳PECVD载板的制备方法,其特征在于,所述步骤9)包括:将所述2D碳/碳复合材料板材放入化学气相沉积炉中,沉积温度为1000~1150℃,通入天然气或丙烷或其它碳氢化合物,以氩气为稀释气体,控制炉压为500~4000Pa,进行10~30h表面热解碳涂层处理。
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CN115215673A (zh) * | 2022-08-02 | 2022-10-21 | 福建康碳复合材料科技有限公司 | 承装石墨负极产品的碳碳复合材料拼接匣钵的制作方法 |
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CN108046821A (zh) * | 2018-01-24 | 2018-05-18 | 航天睿特碳材料有限公司 | 一种多晶硅铸锭炉用碳碳盖板的制备方法 |
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CN115215673A (zh) * | 2022-08-02 | 2022-10-21 | 福建康碳复合材料科技有限公司 | 承装石墨负极产品的碳碳复合材料拼接匣钵的制作方法 |
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