CN113061039A - 一种氮化铝陶瓷发热体的制备方法 - Google Patents
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Abstract
本发明涉及一种氮化铝陶瓷发热体的制备方法,包括:步骤一、一次球磨,在球磨机内加入甲基乙基酮、氮化铝粉体、5wt%的三氧化二钇粉体和三油酸甘油酯连续研磨,得到固体质量分数达到40%以上的一次球磨浆料;步骤二、二次球磨,在球磨机的一次球磨浆料内添加PVB粘结剂和聚环氧乙烯,球磨机继续研磨,直至得到氮化铝流延浆料;步骤三、制备生瓷片,将氮化铝流延浆料注入氮化铝陶瓷发热体模具内;步骤四、除泡;步骤五、将生瓷片从氮化铝陶瓷发热体模具内排出;步骤六、将生瓷片放置在高压条件下,加热至烧结温度1720℃~1820℃,保温时间为3h~5h,形成氮化铝陶瓷发热体。本发明能够提高氮化铝陶瓷发热体的机械强度。
Description
技术领域
本发明涉及陶瓷发热体制备技术领域,尤其涉及一种氮化铝陶瓷发热体的制备方法。
背景技术
陶瓷发热体具备耐腐蚀、耐高温、寿命长、温度均匀和导热性能良好的优点。陶瓷发热体包括电加热丝,以及封装在电加热丝外的陶瓷外壳,电加热丝通电后发热通过陶瓷外壳传导热量以加热物体。
目前陶瓷发热体的陶瓷外壳一般采用氧化铝陶瓷、氧化铍陶瓷或氮化铝陶瓷。其中,氮化铝陶瓷的导热系数可达到150-300W/m·K,是氧化铝陶瓷的7-8倍,超过氧化铍陶瓷的导热系数,氮化铝陶瓷已经逐步取代了氧化铍陶瓷和氮化铝陶瓷应用于陶瓷发热体。
但是本发明人指出,在我国氮化铝陶瓷的商品化、工业化程度并不高,主要原因之一是氮化铝属于共价键化合物,原子自扩散系数小,甚至在制备过程中氮化铝陶瓷存在微小气泡,因此,氮化铝陶瓷很难烧结致密化,即难以获得高的机械强度。
发明内容
因此,针对上述的问题,本发明提出一种氮化铝陶瓷发热体的制备方法,能够提高氮化铝陶瓷发热体的机械强度。
为实现上述目的,本发明采用了以下技术方案:一种氮化铝陶瓷发热体的制备方法,包括以下步骤:
步骤一、一次球磨,在球磨机内以甲基乙基酮为介质,加入氮化铝粉体和5wt%的三氧化二钇粉体连续研磨,并且逐渐添加三油酸甘油酯直至达到氮化铝粉体的饱和吸附;
得到固体质量分数达到40%以上的一次球磨浆料;
步骤二、二次球磨,在球磨机的一次球磨浆料内添加PVB粘结剂和聚环氧乙烯的混合溶液,所述PVB粘结剂和聚环氧乙烯的体积之比为0.9~1.8;并且所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.55~0.6;
所述球磨机继续研磨,直至氮化铝粉体的粒度达到2~3μm,得到氮化铝流延浆料;
步骤三、制备生瓷片,将上述步骤二制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具内,包括以下子步骤:
1)将石蜡覆涂在氮化铝陶瓷发热体模具内壁;
2)在氮化铝陶瓷发热体模具内铺设电加热丝,所述电加热丝包括两个电极端,两个所述电极端延伸到氮化铝陶瓷发热体模具外;
3)步骤二中制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具内,并且氮化铝流延浆料将氮化铝陶瓷发热体模具内的电加热丝完全包覆在内;
步骤四、除泡,将超声波发生器的超声波探头与所述电加热丝的两个电极端接触,通过电加热丝形成高频机械振荡,氮化铝流延浆料内的微小气泡在高频机械振荡下迅速增大,并在脱离氮化铝流延浆料表面破裂,消除氮化铝流延浆料内的微小气泡;
步骤五、待氮化铝陶瓷发热体模具内的氮化铝流延浆料固化成型后形成生瓷片;将氮化铝陶瓷发热体模具浸泡于乙酸乙酯溶液内,直至氮化铝陶瓷发热体模具内壁的石蜡溶解,将生瓷片从氮化铝陶瓷发热体模具内排出;
步骤六、将生瓷片放置在压力为1000MPa~6000MPa的高压条件下,将生瓷片加热至烧结温度1720℃~1820℃,保温时间为3h~5h,形成氮化铝陶瓷发热体;
烧结结束后,先将压力降至标准大气压后,再将氮化铝陶瓷发热体逐渐降温至当前环境温度。
进一步的,所述PVB粘结剂和聚环氧乙烯的体积之比为1。
进一步的,所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.6。
进一步的,所述步骤六中,将生瓷片放置在压力为5000MPa的高压条件下。
进一步的,所述步骤六中,将生瓷片加热至烧结温度1770℃,保温时间为4h。
进一步的,所述步骤六中,生瓷片以20℃/min速率升温至1200℃,而后以10℃/min的速率升温至1770℃。
通过采用前述技术方案,本发明的有益效果是:本氮化铝陶瓷发热体的制备方法通过在一次球磨时加入三油酸甘油酯形成空间位阻效应,改善一次球磨浆料的流动性。而后进行二次球磨,添加PVB粘结剂提高烧结的氮化铝陶瓷发热体的致密度,从而提升其机械强度,添加聚环氧乙烯改善氮化铝陶瓷发热体的柔韧性及延展性。将制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具内,并且电加热丝的两个电极端与超声波探头接触,通过电加热丝形成高频机械振荡,消除氮化铝流延浆料内的微小气泡,提高氮化铝陶瓷发热体的致密度,从而提高氮化铝陶瓷发热体的导热率以及机械强度。而生瓷片放置在压力为1000MPa~6000MPa的高压条件下,将生瓷片加热至烧结温度1720℃~1820℃,保温时间为3h~5h,制备出的高氮化铝陶瓷发热体导热率高、致密度高、机械强度好。优选的,在本技术方案中,将生瓷片放置在压力为5000MPa的高压条件下,且生瓷片以20℃/min速率升温至1200℃,而后以10℃/min的速率升温至1770℃,保温时间为4h,制备出的氮化铝陶瓷发热体导热率和致密度高,也即氮化铝陶瓷发热体的机械强度高。
附图说明
图1是本发明实施例的氮化铝陶瓷发热体模具结构示意图。
具体实施方式
现结合附图和具体实施方式对本发明进一步说明。
参考图1,本实施例提供一种氮化铝陶瓷发热体的制备方法,包括以下步骤:
步骤一、一次球磨,在球磨机内以甲基乙基酮为介质,加入氮化铝粉体和5wt%的三氧化二钇粉体连续研磨,三氧化二钇粉体一方面可以与氮化铝粉体表面氧化形成的氧化铝反应生成较低熔点的第二相,由于液相表面的张力作用,促进氮化铝粉体晶粒的重排,加速烧结体致密化进程,另一方面形成的第二相冷却后,淀析凝结在晶界上,减少了高温下氧进入晶格的可能,起到净化晶格,提高热导率的作用。
并且为了改善一次球磨浆料的流动性,还在球磨机内逐渐添加三油酸甘油酯,由于氮化铝粉体表面可吸附三油酸甘油酯形成空间位阻效应,改善一次球磨浆料的流动性。但是要注意,若三油酸甘油酯添加量不足,则空间位阻效应弱,一次球磨浆料流动性差;而若三油酸甘油酯添加量过多,会导致一次球磨浆料产生絮凝;因此,应当保证逐渐添加三油酸甘油酯直至达到氮化铝粉体的饱和吸附。
得到固体质量分数达到40%以上的一次球磨浆料。
步骤二、二次球磨,在球磨机的一次球磨浆料内添加PVB粘结剂和聚环氧乙烯的混合溶液,通过添加PVB粘结剂和聚环氧乙烯可有效改善制备的氮化铝陶瓷发热体的柔韧性及延展性。
所述PVB粘结剂和聚环氧乙烯的体积之比为0.9~1.8;并且所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.55~0.6,制备出的氮化铝陶瓷发热体的导热率和机械强度高。
更优选的,在本具体实施例中,所述PVB粘结剂和聚环氧乙烯的体积之比为1;并且所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.6。
所述球磨机继续研磨,直至氮化铝粉体的粒度达到2~3μm,得到氮化铝流延浆料。在本具体实施例中,优选的,球磨机研磨氮化铝粉体的粒度达到2μm。
步骤三、制备生瓷片,将上述步骤二制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具1内,图1为所述氮化铝陶瓷发热体模具1结构,所述氮化铝陶瓷发热体模具1上开设有凹槽10;
包括以下子步骤:
1)将石蜡覆涂在氮化铝陶瓷发热体模具1的凹槽10内壁;
2)在氮化铝陶瓷发热体模具1的凹槽10内铺设电加热丝2,所述电加热丝2包括两个电极端20,两个所述电极端20延伸到氮化铝陶瓷发热体模具1外;
3)步骤二中制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具1内,并且氮化铝流延浆料将氮化铝陶瓷发热体模具1内的电加热丝2完全包覆在内。
步骤四、除泡,将超声波发生器的超声波探头与所述电加热丝2的两个电极端20接触,通过电加热丝2形成高频机械振荡,氮化铝流延浆料内的微小气泡在高频机械振荡下迅速增大,并在脱离氮化铝流延浆料表面破裂,消除氮化铝流延浆料内的微小气泡。通过将氮化铝流延浆料内的微小气泡消除,可以提高制备的氮化铝陶瓷发热体密度,提高氮化铝陶瓷发热体的导热率和机械强度。
步骤五、待氮化铝陶瓷发热体模具1内的氮化铝流延浆料固化成型后形成生瓷片;将氮化铝陶瓷发热体模具1浸泡于乙酸乙酯溶液内,直至氮化铝陶瓷发热体模具1的凹槽10内壁的石蜡溶解,将生瓷片从氮化铝陶瓷发热体模具1内排出。
步骤六、将生瓷片放置在压力为1000MPa~6000MPa的高压条件下,将生瓷片加热至烧结温度1720℃~1820℃,保温时间为3h~5h,形成氮化铝陶瓷发热体。
高压能够使得物质间的原子间距压缩,即烧结后的氮化铝晶格常数变小,从而增加生瓷片的致密度,而烧结温度也影响氮化铝陶瓷发热体的致密度和导热率。因此,在本具体实施例中,将生瓷片放置在压力为5000MPa的高压条件下,通过不同的烧结温度下分别得出的几组氮化铝陶瓷发热体的致密度和导热率如下:
烧结温度/(℃) | 1720 | 1745 | 1770 | 1795 | 1820 |
导热率/(W/(m·k)) | 214 | 233 | 248 | 251.5 | 253 |
致密度/(g/c㎡) | 3.14 | 3.17 | 3.30 | 3.30 | 3.31 |
实验证明在烧结温度在1720℃-1770℃范围内,随着烧结温度升高,氮化铝陶瓷发热体的致密度和导热率都有明显的提升;但是在1770℃-1820℃范围内,随着烧结温度升,高氮化铝陶瓷发热体的致密度和导热率并没有明显的提升,烧结温度提高需要投入更多的成本和能源。因此本具体实施例,考虑到成本和能源最优化,优选的,将生瓷片放置在压力为5000MPa的高压条件下,且生瓷片以20℃/min速率升温至1200℃,而后以10℃/min的速率升温至1770℃,保温时间为4h,制备出的氮化铝陶瓷发热体导热率为248W/(m·k)和致密度为3.30g/c㎡,制得的氮化铝陶瓷发热体机械强度较为理想。
待氮化铝陶瓷发热体烧结结束后,先将压力降至标准大气压后,再将氮化铝陶瓷发热体逐渐降温至当前环境温度。
尽管结合优选实施方案具体展示和介绍了本发明,但所属领域的技术人员应该明白,在不脱离所附权利要求书所限定的本发明的精神和范围内,在形式上和细节上可以对本发明做出各种变化,均为本发明的保护范围。
Claims (6)
1.一种氮化铝陶瓷发热体的制备方法,其特征在于,包括以下步骤:
步骤一、一次球磨,在球磨机内以甲基乙基酮为介质,加入氮化铝粉体和5wt%的三氧化二钇粉体连续研磨,并且逐渐添加三油酸甘油酯直至达到氮化铝粉体的饱和吸附;
得到固体质量分数达到40%以上的一次球磨浆料;
步骤二、二次球磨,在球磨机的一次球磨浆料内添加PVB粘结剂和聚环氧乙烯的混合溶液,所述PVB粘结剂和聚环氧乙烯的体积之比为0.9~1.8;并且所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.55~0.6;
所述球磨机继续研磨,直至氮化铝粉体的粒度达到2~3μm,得到氮化铝流延浆料;
步骤三、制备生瓷片,将上述步骤二制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具内,包括以下子步骤:
1)将石蜡覆涂在氮化铝陶瓷发热体模具内壁;
2)在氮化铝陶瓷发热体模具内铺设电加热丝,所述电加热丝包括两个电极端,两个所述电极端延伸到氮化铝陶瓷发热体模具外;
3)步骤二中制备的氮化铝流延浆料注入氮化铝陶瓷发热体模具内,并且氮化铝流延浆料将氮化铝陶瓷发热体模具内的电加热丝完全包覆在内;
步骤四、除泡,将超声波发生器的超声波探头与所述电加热丝的两个电极端接触,通过电加热丝形成高频机械振荡,氮化铝流延浆料内的微小气泡在高频机械振荡下迅速增大,并在脱离氮化铝流延浆料表面破裂,消除氮化铝流延浆料内的微小气泡;
步骤五、待氮化铝陶瓷发热体模具内的氮化铝流延浆料固化成型后形成生瓷片;将氮化铝陶瓷发热体模具浸泡于乙酸乙酯溶液内,直至氮化铝陶瓷发热体模具内壁的石蜡溶解,将生瓷片从氮化铝陶瓷发热体模具内排出;
步骤六、将生瓷片放置在压力为1000MPa~6000MPa的高压条件下,将生瓷片加热至烧结温度1720℃~1820℃,保温时间为3h~5h,形成氮化铝陶瓷发热体;
烧结结束后,先将压力降至标准大气压后,再将氮化铝陶瓷发热体逐渐降温至当前环境温度。
2.根据权利要求1所述的一种氮化铝陶瓷发热体的制备方法,其特征在于:所述PVB粘结剂和聚环氧乙烯的体积之比为1。
3.根据权利要求2所述的一种氮化铝陶瓷发热体的制备方法,其特征在于:所述混合溶液与步骤一中制备的所述一次球磨浆料体积之比为0.6。
4.根据权利要求1或2或3所述的一种氮化铝陶瓷发热体的制备方法,其特征在于:所述步骤六中,将生瓷片放置在压力为5000MPa的高压条件下。
5.根据权利要求4所述的一种氮化铝陶瓷发热体的制备方法,其特征在于:所述步骤六中,将生瓷片加热至烧结温度1770℃,保温时间为4h。
6.根据权利要求5所述的一种氮化铝陶瓷发热体的制备方法,其特征在于:所述步骤六中,生瓷片以20℃/min速率升温至1200℃,而后以10℃/min的速率升温至1770℃。
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