CN117003567A - 一种氮化硅流延生带及其制备方法 - Google Patents
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Abstract
本发明公开了一种氮化硅流延生带及其制备方法，涉及氮化硅流延生带技术领域。本发明氮化硅流延生带所采用的浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体，所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的0.5～3％、4～15％、4～15％和60～80％；所述氮化硅粉的粒径在300nm～1500nm之间。本发明通过调整原料组成以及加工方法，使得显著提高氮化硅流延生带的厚度，同时降低工艺成本以及操作难度，提高氮化硅流延生带的质量。
Description
技术领域
本发明属于一种氮化硅流延生带及其制备方法。
背景技术
随着高性能电子设备及其组件的小型化、集成化，散热已成为其性能和可靠性的关键因素。半导体器件运行产生的热量是导致其失效的关键因素，故对电绝缘陶瓷基板的导热性能提出了更高要求。在这些陶瓷基板中，由于氮化硅具有高热导率、高机械强度和低热膨胀系数、与半导体材料匹配性好等优点，相较于其他基板材料，其具有更优异的综合性能，从而在电力电子器件陶瓷基板制造领域备受关注，目前已在轨道交通、电动汽车、新能源电网、军事及航天等领域得到实际应用。
目前，国内的氮化硅产品主要依赖从国外进口氮化硅流延生带或氮化硅基板。国内对于氮化硅生带的流延浆料配方与制备的研究相对较少。单一的溶剂用量大、且不利于流延浆料在各个干燥温区均匀干燥而导致生带容易开裂，而复杂的溶剂体系有机添加剂较多，环保压力大、成本居高不下。流延生带的厚度也大多局限于0.1～0.25mm之间，需要通过后续的叠层、切片、等静压等工序才能制备符合预期厚度的氮化硅生坯。
发明内容
针对现有技术的不足，本发明提供了一种氮化硅流延生带及其制备方法。本发明通过调整原料组成以及加工方法，使得显著提高氮化硅流延生带的厚度，同时降低工艺成本以及操作难度，提高氮化硅流延生带的质量。
本发明是采用以下技术方案实现的：
一种氮化硅流延生带，所述氮化硅流延生带的浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的0.5～3％、4～15％、4～15％和60～80％；所述氮化硅粉的粒径在300nm～1500nm之间。
优选的，所述分散剂为聚乙烯吡咯烷酮、鱼油、三油酸甘油酯、蓖麻油磷酸酯、磷酸三乙酯中的任意一种或几种的混合物。
优选的，所述增塑剂为邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、邻苯二甲酸丁苄酯、甘油和聚乙二醇中的任意一种或任意几种的混合物。
优选的，所述粘结剂为聚乙烯醇缩丁醛、聚甲基丙烯酸甲酯中的至少一种。
优选的，所述溶剂为小于等于三元的混合溶剂；所述溶剂是由质量比为1:10～10:1醇类、苯类、酮类混合而成；
所述醇类为异丁醇、叔丁醇、苯乙醇、二丙酮醇、正丁醇、乙二醇、异丙醇、丙醇、乙醇中的任意一种；
所述苯类为甲苯、二甲苯中一种；所述酮类为环己酮、丁酮、二丁酮、甲基异丁基酮中的任意一种。
本发明所述氮化硅流延生带的制备方法，包括以下步骤：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置12～24h，得到预溶胶。
(2)将分散剂和溶剂按比例球磨5min-30min，使分散剂充分溶解，然后加入氮化硅粉球磨0.5h-5h，得到一次球磨浆料，所述的一次球磨包括滚筒球磨、搅拌球磨或砂磨中的任意一种或多种组合方式；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨12h～24h，得到二次球磨浆料；
(4)将步骤(3)的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度在2000mPa·s～10000mPa·s之间，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为0.4mm～1.5mm，流延速度为0.1m/min～1.0m/min，将烘箱温度在25～80℃之间设置多级梯度,可流延成型得到厚度在0.1～1mm可调控的氮化硅生带。
与现有技术相比，本发明具有以下有益效果：
(1)本发明采用流延成型技术制备氮化硅生带，流延浆料所用溶剂为小于等于三元的溶剂体系，溶剂挥发速率可调、浆料干燥速度可控、操作简单、成本低廉，利于批量生产。
(2)本发明制备流延浆料采用多级梯度球磨方式，可获得高固相含量的浆料，且可明显改善浆料均匀性，且缩短球磨时间、利于产业化批量生产。
(3)本发明流延成型的氮化硅生带厚度可控，通过控制浆料固相含量与粘度，可一次流延成型目标厚度的氮化硅生带，无需进行叠层等后工序加工便可得到目标厚度的生带，工序更加简单、节省时间、原料与人力成本，利于提高产率，促进批量化生产。
附图说明
图1为实施例1制备的氮化硅流延生带的实物照片；
图2为实施例1所得氮化硅流延生带的断面SEM图；
图3为实施例2所得氮化硅流延生带的实物照片；
图4为实施例2所得氮化硅流延生带的断面SEM图；
图5为实施例3所得氮化硅流延生带的实物照片；
图6为实施例3所得氮化硅流延生带的断面SEM图；
图7为实施例4所得氮化硅流延生带的表面SEM图；
图8为实施例5所得氮化硅流延生带的表面SEM图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种氮化硅流延生带，其浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体，所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的0.5％、12％、9％和65％；
其中，分散剂为鱼油，溶剂为质量比为1:1的乙醇和环己酮；增塑剂为质量比是1:1的邻苯二甲酸二丁酯和聚乙二醇的混合物；粘结剂为聚乙烯醇缩丁醛。
该氮化硅流延生带的制备方法如下：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置18h，得到预溶胶。
(2)将分散剂和溶剂按比例加入到搅拌球磨罐中球磨10min，使分散剂充分溶解，然后加入氮化硅粉，继续球磨1h，得到一次球磨浆料；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨16h，得到二次球磨浆料；
(4)将步骤(3)得到的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度为8000mPa·s，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为1.1mm，流延速度为0.2m/min，在表1所示温度条件下进行流延成型处理，待流延膜烘干后得到厚度为0.45mm的氮化硅流延生带。
表1
| 温区 | 1 | 2 | 3 | 4 | 5 |
| 温度(℃) | 25 | 35 | 45 | 55 | 65 |
实施例1制备的氮化硅流延浆料流动性好，流延生带表面平整、厚度均匀性好，具有较佳的强度和韧性，可轻松脱膜。从图1中可知，本发明的氮化硅流延生带无裂纹、气孔等缺陷生成。由图2可知，氮化硅陶瓷颗粒分布均匀，氮化硅流延生带的微观组织致密。本实施例仅采用两种溶剂，其中无毒无害、价格低廉的乙醇占了很大比重，环己酮为低毒溶剂，整个浆料环境友好、毒性低，成本较低，并且制备工艺简单，具有实现批量生产的潜力。
实施例2
一种氮化硅流延生带，其浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的1％、10％、15％和80％；
其中，分散剂为质量比为1:1的蓖麻油磷酸酯与鱼油混合物，溶剂为质量比为1:1的乙醇和甲苯；增塑剂为邻苯二甲酸二丁酯；粘结剂为聚乙烯醇缩丁醛。
该氮化硅流延生带的制备方法如下：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置18h，得到预溶胶。
(2)将分散剂和溶剂按比例加入到搅拌磨罐中球磨10min，使分散剂充分溶解，然后加入氮化硅粉，继续球磨1h，得到一次球磨浆料；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨16h，得到二次球磨浆料；
(4)将步骤(3)得到的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度为3000mPa·s，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为0.6mm，流延速度为0.5m/min，在表1所示温度条件下进行流延成型处理，待流延膜烘干后得到厚度为0.25mm的氮化硅流延生带。
实施例2制备的氮化硅流延浆料流动性好，流延生带表面平整、厚度均匀性好，具有较佳的强度和韧性，可轻松脱膜。从图3可知，氮化硅流延生带无裂纹、气孔等缺陷生成。由图4可知，氮化硅陶瓷颗粒分布均匀，氮化硅流延生带的微观组织致密。本实施例仅采用两种溶剂，其中无毒无害、价格低廉的乙醇占了很大比重，甲苯价格低廉，在兼顾环境友好的同时进一步降低成本，并且制备工艺简单，具有实现批量生产的潜力。
实施例3
一种氮化硅流延生带，其浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的1.5％、8％、10％和70％；
其中，分散剂为蓖麻油磷酸酯，溶剂为质量比为1:1:1的乙醇、丁酮和二甲苯；增塑剂为邻苯二甲酸二丁酯；粘结剂为聚乙烯醇缩丁醛。
该氮化硅流延生带的制备方法如下：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置18h，得到预溶胶。
(2)将分散剂和溶剂按比例加入到搅拌球磨罐中球磨10min，使分散剂充分溶解，然后加入氮化硅粉，继续球磨1h，得到一次球磨浆料；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨16h，得到二次球磨浆料；
(4)将步骤(3)得到的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度为10000mPa·s，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为1.5mm，流延速度为0.2m/min，在表1所示温度条件下进行流延成型处理，待流延膜烘干后得到厚度为0.75mm的氮化硅流延生带。
本实施例制备的氮化硅流延浆料流动性好，流延生带表面平整、厚度均匀性好，具有较佳的强度和韧性，可轻松脱膜。从图5可知，氮化硅流延生带无裂纹、气孔等缺陷生成。由图6可知，氮化硅陶瓷颗粒分布均匀，氮化硅流延生带的微观组织致密。本实施例仅采用三种溶剂，挥发速率梯度可控，其中无毒无害、价格低廉的乙醇和低毒的丁酮占了很大比重，二甲苯价格低廉，在兼顾环境友好的同时进一步降低成本，并且制备工艺简单，具有实现批量生产的潜力。
实施例4
一种氮化硅流延生带，其浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的1.5％、7％、7％和60％；
其中，分散剂为质量比为1:2的三油酸甘油酯与磷酸三乙酯的混合物，溶剂为质量比为3:3:4的异丙醇、正丁醇与二甲苯的混合物；增塑剂为邻苯二甲酸丁苄酯，粘结剂为质量比为1:1的聚甲基丙烯酸甲酯与聚乙烯醇缩丁醛的混合物。
该氮化硅流延生带的制备方法如下：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置18h，得到预溶胶。
(2)将分散剂和溶剂按比例加入到滚筒球磨罐中球磨30min，使分散剂充分溶解，然后加入氮化硅粉，继续球磨5h，得到一次球磨浆料；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨16h，得到二次球磨浆料；
(4)将步骤(3)得到的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度为2000mPa·s，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为0.5mm，流延速度为0.4m/min，在表1所示温度条件下进行流延成型处理，待流延膜烘干后得到厚度为0.15mm的氮化硅流延生带。
本实施例制备的氮化硅流延浆料流动性好，流延生带表面平整、厚度均匀性好，具有较佳的强度和韧性，可轻松脱膜。从图7可知，氮化硅流延生带无裂纹、气孔等缺陷生成，并且氮化硅陶瓷颗粒分布均匀，氮化硅流延生带的微观组织致密。本实施例仅采用三种溶剂，挥发速率梯度可控，其中低毒低害、价格低廉的异丙醇和正丁醇占了较大比重、正丁醇还可以起到辅助脱泡的作用，二甲苯价格低廉，在兼顾环境友好的同时进一步降低成本，并且制备工艺简单，具有实现批量生产的潜力。
实施例5
一种氮化硅流延生带，其浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的2.5％、8％、5％和65％；
其中，分散剂为磷酸三乙酯，溶剂为质量比3:2的乙醇与二甲苯的混合物；增塑剂为质量比为3:1的邻苯二甲酸丁苄酯与聚已二醇的混合物，粘结剂为聚甲基丙烯酸甲酯。
该氮化硅流延生带的制备方法如下：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置18h，得到预溶胶。
(2)将分散剂和溶剂按比例加入到砂磨机中球磨10min，使分散剂充分溶解，然后加入氮化硅粉，继续球磨50min，得到一次球磨浆料；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨16h，得到二次球磨浆料；
(4)将步骤(3)得到的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度为10000mPa·s，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为1.65mm，流延速度为0.1m/min，在表1所示温度条件下进行流延成型处理，待流延膜烘干后得到厚度为0.85mm的氮化硅流延生带。
本实施例制备的氮化硅流延浆料流动性好，流延生带表面平整、厚度均匀性好，具有较佳的强度和韧性，可轻松脱膜。从图8可知，氮化硅流延生带无裂纹、气孔等缺陷生成。且由图8可知，氮化硅陶瓷颗粒分布均匀，氮化硅流延生带的微观组织致密。本实施例仅采用2种溶剂，种类简单、挥发速率梯度可控，其中无毒无害、价格低廉的乙醇占了很大比重，二甲苯价格低廉，在兼顾环境友好的同时进一步降低成本，并且制备工艺简单，具有实现批量生产的潜力。同时通过调整溶剂、分散剂、增塑剂和粘结剂的组成与搭配，本实施例中所使用的有机物总量明显减少，减少环保压力的同时进一步节约成本。
对比例一
与实施例一基本相同，不同点在于，所用溶剂仅为无水乙醇，溶剂用量为无机相粉体质量的140％，所制得的氮化硅流延生带厚度为0.445mm，但生带容易开裂。
对比例二
与实施例三基本相同，不同点在于所用溶剂为质量比为1:1:1的丁酮、环己酮、甲基异丁基酮，溶剂用量为无机相粉体质量的150％，所制得氮化硅流延生带厚度为0.24mm。
在对比例一中，仅使用乙醇作为溶剂，使分散剂的溶解性和分散效果降低，故需要更多的溶剂以获得分散效果较好的一次球磨浆料，且单一溶剂的沸点单一，挥发速率不可调控，生带容易开裂。
在对比例二中，使用沸点不同的三种酮作为溶剂，浆料挥发速率可调控，生带不易开裂。虽然单一的酮类溶剂利于分散剂对氮化硅粉体的分散作用，但聚乙烯醇缩丁醛在酮类溶剂中的溶解性较低，故需要更多的酮类溶剂以制备预溶胶体。
需要说明的是，以上列举的仅是本发明的若干个具体实施例，显然本发明不仅仅限于以上实施例，还可以有其他变形。本领域的技术人员从本发明公开内容直接导出或间接引申的所有变形，均应认为是本发明的保护范围。
Claims (6)
1.一种氮化硅流延生带，其特征在于，所述氮化硅流延生带的浆料原料由无机相和有机相组成，所述无机相为氮化硅粉体；所述有机相由分散剂、增塑剂、粘结剂和溶剂组成，其含量分别为无机相粉体质量的0.5～3％、4～15％、4～15％和60～80％；所述氮化硅粉的粒径在300nm～1500nm之间。
2.根据权利要求1所述氮化硅流延生带，其特征在于，所述分散剂为聚乙烯吡咯烷酮、鱼油、三油酸甘油酯、蓖麻油磷酸酯、磷酸三乙酯中的任意一种或几种的混合物。
3.根据权利要求1所述氮化硅流延生带，其特征在于，所述增塑剂为邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、邻苯二甲酸丁苄酯、甘油和聚乙二醇中的任意一种或任意几种的混合物。
4.根据权利要求1所述氮化硅流延生带，其特征在于，所述粘结剂为聚乙烯醇缩丁醛、聚甲基丙烯酸甲酯中的至少一种。
5.根据权利要求1所述氮化硅流延生带，其特征在于，所述溶剂为小于等于三元的混合溶剂；所述溶剂是由质量比为1:10～10:1醇类、苯类、酮类混合而成；
所述醇类为异丁醇、叔丁醇、苯乙醇、二丙酮醇、正丁醇、乙二醇、异丙醇、丙醇、乙醇中的任意一种；
所述苯类为甲苯、二甲苯中一种；所述酮类为环己酮、丁酮、二丁酮、甲基异丁基酮中的任意一种。
6.根据权利要求1～5任意一项所述氮化硅流延生带的制备方法，其特征在于，包括以下步骤：
(1)将粘结剂和增塑剂加入溶剂中充分搅拌、溶解后静置12～24h，得到预溶胶；
(2)将分散剂和溶剂按比例球磨5min-30min，使分散剂充分溶解，然后加入氮化硅粉球磨0.5h-5h，得到一次球磨浆料，所述的一次球磨包括滚筒球磨、搅拌球磨或砂磨中的任意一种或多种组合方式；
(3)将一次球磨浆料和预溶胶加入到滚筒球磨罐中，继续球磨12h～24h，得到二次球磨浆料；
(4)将步骤(3)的二次球磨浆料进行真空脱泡处理，控制脱泡后的浆料粘度在2000mPa·s～10000mPa·s之间，将脱泡后的浆料倒入流延机料槽，调整刮刀高度为0.4mm～1.5mm，流延速度为0.1m/min～1.0m/min，将烘箱温度在25～80℃之间设置多级梯度,可流延成型得到厚度在0.1～1mm可调控的氮化硅生带。
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