CN113526962A - 一种轧膜成型工艺生产氮化物陶瓷基板的方法 - Google Patents

一种轧膜成型工艺生产氮化物陶瓷基板的方法 Download PDF

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CN113526962A
CN113526962A CN202110858848.8A CN202110858848A CN113526962A CN 113526962 A CN113526962 A CN 113526962A CN 202110858848 A CN202110858848 A CN 202110858848A CN 113526962 A CN113526962 A CN 113526962A
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林伟毅
陈智
刘卫平
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Fujian Zhenjing New Material Technology Co ltd
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Abstract

本发明公开了一种轧膜成型工艺生产氮化物陶瓷基板的方法，S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS‑1071耐高温无机粘合剂，用球磨方式进行第一次混合；所述烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:0.5～1:3；所述烧结助剂和氮化硅粉的质量比为1:10～1:40，所述ZS‑1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成；S2，混炼：采用混炼机进行混炼，ZS‑1071耐高温无机粘合剂与氮化硅粉均匀混合；S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；通过真空脱泡机对胚体进行脱泡，增加胚体的密度，保证产品的质量，且通过ZS‑1071耐高温无机粘合剂与烧结助剂配合，增加胚体整体的韧性，进而保证装置的使用寿命。

Description

一种轧膜成型工艺生产氮化物陶瓷基板的方法
技术领域
本发明涉及氮化物陶瓷基板生产技术领域，具体为一种轧膜成型工艺生产氮化物陶瓷基板的方法。
背景技术
氮化物陶瓷是氮与金属或非金属元素造成的陶瓷，是一类重要的结构与功能材料，具有良好的力学、化学、电学、热学及高温物理性能，在冶金、航空、化工、陶瓷、电子、机械及半导体等行业具有广泛的应用。氮化硅、氮化硼、氮化铝、氮化镓、氮化钛及过渡金属氮化物是研究与应用的热点。
氮化物陶瓷基板生产多用到流延成型法和挤膜成型法这两种成型方法，其批量生产的能力非常高，但是用这两种成型方法制成的薄型压电陶瓷片致密度差，从而导致产品的绝缘电阻大大降低，甚至出现短路情况，且现有通过流延成型法和挤膜成型的陶瓷基板，其韧性较差。
发明内容
(一)解决的技术问题
针对现有技术的不足，本发明提供了一种轧膜成型工艺生产氮化物陶瓷基板的方法，解决了上述背景技术中的问题。
(二)技术方案
基于背景技术存在的技术问题，本发明提出一种轧膜成型工艺生产氮化物陶瓷基板的方法，包括如下步骤：
S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS-1071耐高温无机粘合剂，用球磨方式进行第一次混合；所述烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:0.5～1:3；所述烧结助剂和氮化硅粉的质量比为1:10～1:40，所述ZS-1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成；
S2，混炼：采用混炼机进行混炼，ZS-1071耐高温无机粘合剂与氮化硅粉均匀混合；
S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；
S4，将脱泡处理后的浆料用流延成型的方法制备出薄片状素坯；
S5，将薄片状素坯置于排胶炉中进行排胶处理；
S6、粗轧：将步骤S5所得坯料置将于两辊粗轧机上正转，转速调节为5r/min～8r/min，经过折迭、倒向、反复进行粗轧，坯料轧至表面不黏手、不粘辊、无气泡、然后修去边缘裂口；
S7、中轧：将步骤S5所得坯片经过中轧机辊轧；
S8、在坯片的表面涂抹纳米陶瓷粉；
S9、精轧：采用两台两辊轧膜机级联进行精轧，两台两辊精轧机正转；
S10、将排胶后的素坯置于高温烧结炉中进行烧结，得到氮化硅陶瓷基板；在高温烧结前先在真空条件下，加热至1000～1400℃后，保温3～5小时；然后，在1～10MPa的氮气压力下，继续加热至1800～1900℃，保温5～20小时烧结而成。
S11、然后根据需求对胚料进行裁切得到所需大小的坯片。
S12、然后在胚体的表面钻上通道孔，采用通过磁控溅射，图形化光刻，干法湿法蚀刻，电镀加厚工艺，在陶瓷基板上制作出超细线条电路图形。
优选的，所述的步骤S6包括以下步骤：打开混炼机，调节转速为8r/min～15r/min，将步骤S1所得浆料用料铲加入运转中的混炼机的轧辊上，将接料桶置于出料口处，循环碾压10次～15次。
优选的，所述的步骤S7包括以下步骤：打开两辊中轧机，压延机正转，调节转速为15r/min～25r/min，两侧辊距调至8mm，将坯片一端垂直放入两辊筒中间，从另一端辊筒上拉出坯片，再倒向后垂直放入压延机两轧辊间碾压，重复操作3次～5次。
优选的，所述S7的步骤包括以下步骤：将中轧二所得坯片在第一精轧机上轧膜2次～3次，测量厚度。
优选的，所述聚乙烯醇粘合剂通过将17-88型聚乙烯醇18份、去离子水73份、甘油2份和无水乙醇7份倒入搅拌机中搅拌形成混合液，同时加热到90℃，待17-88型聚乙烯醇完全溶解，将上述混合液趁热过40目筛制得。
优选的，所述排胶处理为在真空条件下，在400～600℃的温度下，保温5～10小时。
(三)有益效果
本发明提供了一种轧膜成型工艺生产氮化物陶瓷基板的方法。具备以下有益效果：S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS-1071耐高温无机粘合剂，用球磨方式进行第一次混合；烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:0.5～1:3；烧结助剂和氮化硅粉的质量比为1:10～1:40，ZS-1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成，ZS-1071耐高温无机粘合剂和氮化硅粉的质量比为1:100～1:500；S2，混炼：采用混炼机进行混炼，ZS-1071耐高温无机粘合剂与氮化硅粉均匀混合；S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；S4，将脱泡处理后的浆料用流延成型的方法制备出薄片状素坯；S5，将薄片状素坯置于排胶炉中进行排胶处理；S6、粗轧：将步骤S5所得坯料置将于两辊粗轧机上正转，转速调节为5r/min～8r/min，经过折迭、倒向、反复进行粗轧，坯料轧至表面不黏手、不粘辊、无气泡、然后修去边缘裂口；S7、中轧：将步骤S5所得坯片经过中轧机辊轧；S8、在坯片的表面涂抹纳米陶瓷粉；S9、精轧：采用两台两辊轧膜机级联进行精轧，两台两辊精轧机正转，精轧机一辊筒速比为1:1.5～2，精轧机二辊筒速比为1:1～1.3，精轧机的辊距调节至0.2-5mm；S10、将排胶后的素坯置于高温烧结炉中进行烧结，得到氮化硅陶瓷基板；在高温烧结前先在真空条件下，加热至1000～1400℃后，保温3～5小时；然后，在1～10MPa的氮气压力下，继续加热至1800～1900℃，保温5～20小时烧结而成；S11、然后根据需求对胚料进行裁切得到所需大小的坯片；S12、然后在胚体的表面钻上通道孔，采用通过磁控溅射，图形化光刻，干法湿法蚀刻，电镀加厚工艺，在陶瓷基板上制作出超细线条电路图形，通过真空脱泡机对胚体进行脱泡，增加胚体的密度，保证产品的质量，且通过ZS-1071耐高温无机粘合剂与烧结助剂配合，增加胚体整体的韧性，进而保证装置的使用寿命。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例提供两种技术方案：一种轧膜成型工艺生产氮化物陶瓷基板的方法，具体包括以下实施例：
实施例1
S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS-1071耐高温无机粘合剂，用球磨方式进行第一次混合；烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:0.5；烧结助剂和氮化硅粉的质量比为1:10，ZS-1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成，ZS-1071耐高温无机粘合剂和氮化硅粉的质量比为1:100；
S2，混炼：采用混炼机进行混炼，ZS-1071耐高温无机粘合剂与氮化硅粉均匀混合；
S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；
S4，将脱泡处理后的浆料用流延成型的方法制备出薄片状素坯；
S5，将薄片状素坯置于排胶炉中进行排胶处理；
S6、粗轧：将步骤S5所得坯料置将于两辊粗轧机上正转，转速调节为5r/min，经过折迭、倒向、反复进行粗轧，坯料轧至表面不黏手、不粘辊、无气泡、然后修去边缘裂口；
S7、中轧：将步骤S5所得坯片经过中轧机辊轧；
S8、在坯片的表面涂抹纳米陶瓷粉；
S9、精轧：采用两台两辊轧膜机级联进行精轧，两台两辊精轧机正转，精轧机一辊筒速比为1:1.5～2，精轧机二辊筒速比为1:1，精轧机的辊距调节至1mm；
S10、将排胶后的素坯置于高温烧结炉中进行烧结，得到氮化硅陶瓷基板；在高温烧结前先在真空条件下，加热至1000℃后，保温3小时；然后在1MPa的氮气压力下，继续加热至1800℃，保温5小时烧结而成；
S11、然后根据需求对胚料进行裁切得到所需大小的坯片；
S12、然后在胚体的表面钻上通道孔，采用通过磁控溅射，图形化光刻，干法湿法蚀刻，电镀加厚工艺，在陶瓷基板上制作出超细线条电路图形。
实施例2
S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS-1071耐高温无机粘合剂，用球磨方式进行第一次混合；烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:3；烧结助剂和氮化硅粉的质量比为1:40，ZS-1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成，ZS-1071耐高温无机粘合剂和氮化硅粉的质量比为1:500；
S2，混炼：采用混炼机进行混炼，ZS-1071耐高温无机粘合剂与氮化硅粉均匀混合；
S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；
S4，将脱泡处理后的浆料用流延成型的方法制备出薄片状素坯；
S5，将薄片状素坯置于排胶炉中进行排胶处理；
S6、粗轧：将步骤S5所得坯料置将于两辊粗轧机上正转，转速调节为8r/min，经过折迭、倒向、反复进行粗轧，坯料轧至表面不黏手、不粘辊、无气泡、然后修去边缘裂口；
S7、中轧：将步骤S5所得坯片经过中轧机辊轧；
S8、在坯片的表面涂抹纳米陶瓷粉；
S9、精轧：采用两台两辊轧膜机级联进行精轧，两台两辊精轧机正转，精轧机一辊筒速比为1:2，精轧机二辊筒速比为1:1.3，精轧机的辊距调节至5mm；
S10、将排胶后的素坯置于高温烧结炉中进行烧结，得到氮化硅陶瓷基板；在高温烧结前先在真空条件下，加热至1400℃后，保温5小时；然后在10MPa的氮气压力下，继续加热至1900℃，保温20小时烧结而成；
S11、然后根据需求对胚料进行裁切得到所需大小的坯片；
S12、然后在胚体的表面钻上通道孔，采用通过磁控溅射，图形化光刻，干法湿法蚀刻，电镀加厚工艺，在陶瓷基板上制作出超细线条电路图形。
效果实施例
某氮化物陶瓷基板加工工厂，分别采用实施例1-2的加工工艺，在加工完成后，采用实施例1-2陶瓷基板加工工艺其密度为2.05g/cm3，采用普通抛光工艺加工的机电设备其表面平面度在2.5g/cm3以上，采用实施例1-2氮化物陶瓷基板成型工艺，保证成型陶瓷基板的密度和韧性。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (6)

1.一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，包括如下步骤：
S1、配料：将氮化硅粉、烧结助剂、聚乙烯醇粘合剂、ZS-1071耐高温无机粘合剂，用球磨方式进行第一次混合；所述烧结助剂为稀土氧化物和氧化镁的混合物，稀土氧化物和氧化镁的质量比为1:0.5～1:3；所述烧结助剂和氮化硅粉的质量比为1:10～1:40，所述ZS-1071耐高温无机粘合剂由无机纳米材料经缩聚反应制成，ZS-1071耐高温无机粘合剂和氮化硅粉的质量比为1:100～1:500；
S2，混炼：采用混炼机进行混炼，ZS-1071耐高温无机粘合剂与氮化硅粉均匀混合；
S3，脱泡：将浆料倒入容器，置于真空脱泡机中进行脱泡处理；
S4，将脱泡处理后的浆料用流延成型的方法制备出薄片状素坯；
S5，将薄片状素坯置于排胶炉中进行排胶处理；
S6、粗轧：将步骤S5所得坯料置将于两辊粗轧机上正转，转速调节为5r/min～8r/min，经过折迭、倒向、反复进行粗轧，坯料轧至表面不黏手、不粘辊、无气泡、然后修去边缘裂口；
S7、中轧：将步骤S5所得坯片经过中轧机辊轧；
S8、在坯片的表面涂抹纳米陶瓷粉；
S9、精轧：采用两台两辊轧膜机级联进行精轧，两台两辊精轧机正转，精轧机一辊筒速比为1:1.5～2，精轧机二辊筒速比为1:1～1.3，所述精轧机的辊距调节至0.2-5mm；
S10、将排胶后的素坯置于高温烧结炉中进行烧结，得到氮化硅陶瓷基板；在高温烧结前先在真空条件下，加热至1000～1400℃后，保温3～5小时；然后，在1～10MPa的氮气压力下，继续加热至1800～1900℃，保温5～20小时烧结而成；
S11、然后根据需求对胚料进行裁切得到所需大小的坯片；
S12、然后在胚体的表面钻上通道孔，采用通过磁控溅射，图形化光刻，干法湿法蚀刻，电镀加厚工艺，在陶瓷基板上制作出超细线条电路图形。
2.根据权利要求1所述一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，所述的步骤S6包括以下步骤：打开混炼机，调节转速为8r/min～15r/min，将步骤S1所得浆料用料铲加入运转中的混炼机的轧辊上，将接料桶置于出料口处，循环碾压10次～15次。
3.根据权利要求1所述一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，所述的步骤S7包括以下步骤：打开两辊中轧机，压延机正转，调节转速为15r/min～25r/min，两侧辊距调至8mm，将坯片一端垂直放入两辊筒中间，从另一端辊筒上拉出坯片，再倒向后垂直放入压延机两轧辊间碾压，重复操作3次～5次。
4.根据权利要求1所述一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，所述S7的步骤包括以下步骤：将中轧二所得坯片在第一精轧机上轧膜2次～3次，测量厚度。
5.根据权利要求1所述一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，所述聚乙烯醇粘合剂通过将17-88型聚乙烯醇18份、去离子水73份、甘油2份和无水乙醇7份倒入搅拌机中搅拌形成混合液，同时加热到90℃，待17-88型聚乙烯醇完全溶解，将上述混合液趁热过40目筛制得。
6.根据权利要求1所述一种轧膜成型工艺生产氮化物陶瓷基板的方法，其特征在于，所述排胶处理为在真空条件下，在400～600℃的温度下，保温5～10小时。
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