CN115286398A - 大型薄壁氮化硅结构件及其烧结方法 - Google Patents
大型薄壁氮化硅结构件及其烧结方法 Download PDFInfo
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Abstract
本发明公开了大型薄壁氮化硅结构件及其烧结方法,属于氮化硅陶瓷烧结技术领域,其技术方案要点是,步骤如下:S1、制备氮化硅造粒粉;S2、氮化硅造粒粉经过等静压成型,制成生坯;S3、在生坯内壁嵌入氮化硅陶瓷管,生坯内壁和氮化硅陶瓷管的外壁之间嵌有多个弹性定位件,形成插芯烧结组件;然后对其进行烧结;S4、获得大型氮化硅陶瓷薄壁管。本发明成功制备出了高度>200mm、直径>100mm、壁厚<2mm、变形量<0.2mm、抗弯强度≥750Mpa的大型氮化硅陶瓷薄壁管;该方式能够使生坯在烧结过程中定向收缩,便于实现对产品形状和尺寸的精准性预测和控制、减少加工成本、降低加工废料排放量、提高使用寿命和经济效益。
Description
技术领域
本发明涉及氮化硅陶瓷烧结技术领域,尤其涉及大型薄壁氮化硅结构件及其烧结方法。
背景技术
氮化硅烧结过程属于液相烧结,烧结过程中伴随着一定的收缩。因此对于大型薄壁氮化硅管(高度>200mm,外径>100mm,壁厚小于2mm),烧结时径向方向极易变形(通常变形量>2mm);传统制备方式对于大型薄壁氮化硅唯有烧结前加大其生坯壁厚,烧结完成后通过后期机加工将多余的部分加工掉(加工余量大于5mm),才能达到产品所需尺寸及要求。
但由于氮化硅陶瓷硬度极高,其硬度仅次于金刚石等超硬材料,因此增大余量的烧结方式会导致后期加工成本严重增加,且加工废料会对环境造成很大的污染;同时,较大的加工余量会造成产品内部机械损伤,及过多的残余应力,严重影响氮化硅陶瓷的使用寿命。
为了解决上述问题,在现有技术的基础上提供了大型薄壁氮化硅结构件及其烧结方法。
发明内容
本发明的目的是提供大型薄壁氮化硅结构件及其烧结方法,该方法成功制备出了高度>200mm、直径>100mm、壁厚<2mm、且变形量<0.2mm、抗弯强度≥750MPa的大型氮化硅陶瓷薄壁管;并且,该方法摒弃了大型氮化硅陶瓷薄壁管传统的烧结方式,采用插芯烧结的方式,在插芯烧结的过程中,通过氮化硅陶瓷管插芯和石墨纸,能够使目标产品在烧结过程中实现定向收缩和变形,便于实现对产品形状和尺寸的精准性预测和控制,从而能够获得优异的产品良率;此外,该方法制备得到的大型氮化硅陶瓷薄壁管,无需加工余量,减少了加工成本,降低了加工废料的排放,提高了氮化硅陶瓷使用寿命;因此,本方法增加了经济效益,还有效避免了因传统烧结导致的环境污染问题。
本发明的上述技术目的是通过以下技术方案得以实现的:
大型薄壁氮化硅结构件的烧结方法,包括:
S1、将原料经过球磨、喷雾造粒,制成氮化硅造粒粉;
S2、步骤S1所述的氮化硅造粒粉经过等静压成型,制成生坯;
S3、在步骤S2所述的生坯内壁嵌入氮化硅陶瓷管作为插芯,且所述生坯的内壁和氮化硅陶瓷管的外壁之间还嵌有多个弹性定位件,形成插芯烧结组件;然后对所述插芯烧结组件进行烧结;
S4、烧结完成后,依次将弹性定位件、插芯取出,即可获得大型氮化硅陶瓷薄壁管。
进一步地,步骤S1中,所述原料包括氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉和氮化钛粉。
进一步地,所述氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为80~90%:3~10%:3~10%:1~5%:1~5%。
进一步地,所述弹性定位件为石墨纸。
进一步地,步骤S3中,多张所述石墨纸沿所述氮化硅陶瓷管的外周均匀分布。
进一步地,每2张相邻的石墨纸之间的间距为10mm。
进一步地,步骤S3中,烧结温度为1700~1780℃,保温时间为1.5~4h,压力为2~6MPa。
本发明还提供了大型薄壁氮化硅结构件,根据权利要求1-5任意一项所述的大型薄壁氮化硅结构件的烧结方法制得大型氮化硅陶瓷薄壁管。
进一步地,所述大型氮化硅陶瓷薄壁管的高度>200mm、直径>100mm、壁厚<2mm、且内外径变形量<0.2mm。
通过采用上述技术方案,在生坯内壁嵌入氮化硅陶瓷管作为插芯,由于氮化硅陶瓷管插芯的壁厚较大,且氮化硅陶瓷管的在烧结过程中收缩变形量小,因此,氮化硅陶瓷管能够有效控制外部生坯的定向收缩和变形。
在相同烧结环境下,不同尺寸的同类产品存在着一定的烧结收缩差异,采用纯度>99.99%的高纯石墨纸,由于石墨纸存在着一定的弹性,并且具有优异的耐高温特性,因此在大型氮化硅陶瓷薄壁管与内部插芯收缩的同时,在生坯的内壁和氮化硅陶瓷管的外壁之间嵌设多张石墨纸,能够有效避免因生坯和氮化硅陶瓷管之间的收缩差异导致的产品涨裂;同时,石墨纸能够起到定位的作用,能够更好的进行定向收缩。
综上所述,本发明具有以下有益效果:
1.本发明成功制备出了高度>200mm、直径>100mm、壁厚<2mm、且变形量<0.2mm的大型氮化陶瓷硅薄壁管,该大型氮化硅陶瓷薄壁管的抗弯强度≥750MPa。
2.本发明摒弃了大型氮化硅陶瓷薄壁管传统的烧结方式,采用插芯烧结的方式,在插芯烧结的过程中,通过氮化硅陶瓷管插芯和石墨纸,能够使目标产品在烧结过程中实现定向收缩和变形,便于实现对产品形状和尺寸的精准性预测和控制,从而能够获得优异的产品良率。
3.本发明制备得到的大型氮化硅陶瓷薄壁管,无需加工余量,减少了加工成本,降低了加工废料的排放,提高了氮化硅陶瓷使用寿命;因此,本方法增加了经济效益,还有效避免了因传统烧结导致的环境污染问题。
附图说明
图1是本发明实施例的整体结构示意图;
图2是本发明实施例的剖面结构示意图;
图3是本发明实施例的产品示意图;
图4是本发明对比例的产品示意图。
图中:1、氮化硅陶瓷管;2、石墨纸;3、大型氮化硅陶瓷薄壁管。
具体实施方式
下面结合附图和实施方式对本发明作进一步的详细说明:
实施例1:大型薄壁氮化硅结构件的烧结方法,包括如下步骤:
S1、将氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉和氮化钛粉经过球磨、喷雾造粒,制成氮化硅造粒粉;氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为80:10%:3%:5%:2%。
S2、步骤S1的氮化硅造粒粉经过等静压成型,制成生坯,生坯的尺寸为D122×D117×250mm,烧结后产品的期望目标尺寸为D100×D96×205。
S3、在步骤S2的生坯内壁嵌入氮化硅陶瓷管作为插芯,插芯的尺寸为D115×D95×250mm,且生坯的内壁和氮化硅陶瓷管的外壁之间存在1mm的间隙,生坯的内壁和氮化硅陶瓷管的外壁之间填充有多张10×250mm、厚度为1mm的石墨纸,石墨纸采用纯度>99.99%的高纯石墨纸,形成插芯烧结组件;然后对插芯烧结组件进行烧结。
多张石墨纸沿氮化硅陶瓷管的外周均匀分布,每2张相邻的石墨纸之间的间距为10mm,烧结温度为1700℃,保温时间为1.5h,压力为2MPa。
S4、烧结完成后,依次将石墨纸、插芯取出,即可获得大型氮化硅陶瓷薄壁管。
实施例2:与实施例1的不同之处在于:步骤S1中,氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为90%:3%:3%:1%:3%;步骤S3中,烧结温度为1780℃,保温时间为4h,压力为6MPa。
实施例3:与实施例1的不同之处在于:步骤S1中,氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为81%:3%:10%:1%:5%;步骤S3中,烧结温度为1730℃,保温时间为2.5h,压力为4MPa。
实施例4:与实施例1的不同之处在于:步骤S1中,氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为85%:6%:6%:3%:1%;步骤S3中,烧结温度为1760℃,保温时间为3.5h,压力为5MPa。
实验结果:实施例1-4烧结完成后大型氮化硅陶瓷薄壁管的抗弯强度均≥750MPa;烧结后的实际尺寸为(D99.80-100.18)×(D94.82-95.09)×205;插芯烧结完成后内外径变形量约为±0.18mm。(内外径变形量:内径和外径与预设的烧结后尺寸的偏差量)。
对比例:大型薄壁氮化硅结构件的烧结方法,包括如下步骤:
S1、将氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉和氮化钛粉经过球磨、喷雾造粒,制成氮化硅造粒粉;氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为80:10%:3%:5%:2%。
S2、步骤S1的氮化硅造粒粉经过等静压成型,制成生坯,生坯的尺寸为D122×D117×250mm,烧结后产品的期望目标尺寸为D100×D96×205。
S3、将步骤S2的生坯进行传统的立放烧结,烧结温度为1700℃,保温时间为1.5h,压力为2MPa。
S4、烧结完成后,获得大型氮化硅陶瓷薄壁管。
对比例结果:大型氮化硅陶瓷薄壁管的实际尺寸为D(97.8-102.2)×D(93.8-98.2)×205;烧结完成后内外径变形量约为±2.2mm。
总结:大型氮化硅陶瓷管的传统烧结方式是需要加大生坯余量后进行烧结,由于传统烧结方式得到的产品变形量非常大,生坯烧结前需要规划较多的余量,烧结完成后通过后期机加工将多余的部分加工掉,才能达到产品所需尺寸及要求;加工余量还会衍生出环境污染、生产成本增加、机械损伤等一系列的问题;并且,由于其烧结前后内外径变形量大的特点,还容易出现如图4所示的产品变形问题,降低了产品的生产良率。
本发明的方法,烧结完成后的内外径变形量远远低于传统烧结方式,产品基本如图3所示,能够有效实现产品形状和尺寸的精准性预测和控制,从而能够获得优异的产品良率;并且,此方法无需加工余量,能够有效避免因加工余量导致的问题。
本具体实施例仅仅是对本发明的解释,其并不是对本发明的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本发明的权利要求范围内都受到专利法的保护。
Claims (9)
1.大型薄壁氮化硅结构件的烧结方法,其特征是,包括如下步骤:
S1、将原料经过球磨、喷雾造粒,制成氮化硅造粒粉;
S2、步骤S1所述的氮化硅造粒粉经过等静压成型,制成生坯;
S3、在步骤S2所述的生坯内壁嵌入氮化硅陶瓷管作为插芯,且所述生坯的内壁和氮化硅陶瓷管的外壁之间还嵌有多个弹性定位件,形成插芯烧结组件;然后对所述插芯烧结组件进行烧结;
S4、烧结完成后,依次将弹性定位件、插芯取出,即可获得大型氮化硅陶瓷薄壁管。
2.根据权利要求1所述的大型薄壁氮化硅结构件的烧结方法,其特征是:步骤S1中,所述原料包括氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉和氮化钛粉。
3.根据权利要求2所述的大型薄壁氮化硅结构件的烧结方法,其特征是:所述氮化硅粉、氧化铝粉、氧化钇粉、碳化钛粉、氮化钛粉的原料添加重量比为80~90%:3~10%:3~10%:1~5%:1~5%。
4.根据权利要求1所述的大型薄壁氮化硅结构件的烧结方法,其特征是:所述弹性定位件为石墨纸。
5.根据权利要求4所述的大型薄壁氮化硅结构件的烧结方法,其特征是:步骤S3中,多张所述石墨纸沿所述氮化硅陶瓷管的外周均匀分布。
6.根据权利要求5所述的大型薄壁氮化硅结构件的烧结方法,其特征是:每2张相邻的石墨纸之间的间距为10mm。
7.根据权利要求6所述的大型薄壁氮化硅结构件的烧结方法,其特征是:步骤S3中,烧结温度为1700~1780℃,保温时间为1.5~4h,压力为2~6MPa。
8.大型薄壁氮化硅结构件,其特征是:根据权利要求1-7任意一项所述的大型薄壁氮化硅结构件的烧结方法制得大型氮化硅陶瓷薄壁管。
9.根据权利要求8所述的大型薄壁氮化硅结构件,其特征是:所述大型氮化硅陶瓷薄壁管的高度>200mm、直径>100mm、壁厚<2mm、且内外径变形量<0.2mm。
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