CN111548153A - 一种陶瓷种植体的制备方法 - Google Patents
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Abstract
本发明公开了一种陶瓷种植体的制备方法,采用的造粒粉A和造粒粉B的主要成分均为3mol%钇稳定氧化锆粉,区别为在作为表面材料的造粒粉B中添加了颗粒状造孔剂,所以造粒粉A和造粒粉B的结合性好,通过分层加料后,可同步成型,烧结制得的种植体既能保持氧化锆良好的力学性能,又能保证种植体牙根部表面具有人体牙根相近的孔隙,克服了喷涂、喷丸处理工艺制备的种植体表面与主体结合不牢固及喷砂工艺制备的种植体对孔隙控制性差的缺点。
Description
技术领域
本发明涉及牙科种植体领域,具体涉及一种陶瓷种植体的制备方法。
背景技术
缺牙修复目前主要有三种方法,即活动假牙、烤齿牙和种植牙。活动假牙简单、便宜,但舒适度、美观度和咀嚼效果都非常差。烤齿牙是较好的修复方式,但缺少一颗牙就要把两边的健康牙磨掉,且没有牙根刺激作用,牙槽会慢慢萎缩。种植牙是目前兼美观和功能性最好的牙列缺损修复的方式之一。
随着生活水平和审美要求的不断提高,种植义齿修复已成为口腔修复的重要组成部分。原有钛种植体由于伪影、色泽、种植体周围炎等问题,氧化锆种植体成为种植体发展的趋势。氧化锆作为种植体牙根材料具有良好的生物相容性和物理性能,经过合理的外科手术将植体植入颌骨,可以形成种植体与骨组织在分子水平上的结合,在生理性质咬合力的作用下,有活化的细胞在起作用,动态矿化,改进植体的稳定性。这种结合是生理性的,利用的是口腔组织的再生和愈合能力,具体来说,种植体植入颌骨后,会依靠分化中的骨细胞向种植体表面迁移、黏附、增殖和分化,并对种植体表面进行改造。随后向成骨细胞分化,成骨细胞分泌大量基质和生长因子并继而发生钙化,参与骨的重建。这就要求氧化锆种植体既骨有良好的稳定性,合适的硬度和弹性模量、较高的力学性能和韧性,同时表面需有良好的孔隙。
为了提高种植体表面粗糙度,其表面改性处理有多种类型,包括喷涂、喷砂、酸蚀和激光刻蚀等,但这些表面改性处理方法仍存在许多不足。当种植体植入到口腔中后,在力学环境和生物液体侵蚀的共同作用下,涂层容易脱落、溶解,造成材料的生物活性降低、使用寿命缩短。此外,由于种植体的硬度较高,采用喷砂、酸蚀和激光刻蚀的方法不仅成孔难度较大,对种植体的孔隙控制性也较差,口腔组织与种植体的结合性较低。
发明内容
本发明的目的在于提供一种陶瓷种植体的制备方法,采用不同原料组分,分层加料,同步成型,烧结制得的种植体既能保持氧化锆良好的力学性能,又能保证种植体牙根部表面具有人体牙根相近的孔隙,克服了喷涂、喷丸处理工艺制备的种植体表面与主体结合不牢固及喷砂工艺制备的种植体对孔隙控制性差的缺点。
为实现上述目的,本发明采用以下技术方案:
一种陶瓷种植体的制备方法,包括以下步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.06-0.15mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉60-80份、造孔剂20-40份混合均匀,再经过造粒机制成粒径为0.06-0.15mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,表面层的厚度为总厚度的20%-25%,经干压或冷等静压成型后得到毛坯,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,素坯经过分段升温后,在1500-1530℃的温度条件下保温40-90min,得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡3-5h,然后20%NaHCO3溶液浸泡1~2h,最后用去离子水清洗;
S5、杀菌:将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
优选地,步骤S2中的双层加料方法具体为:采用具有同心加料口的双层加料漏斗,先将双层加料漏斗伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗的中间加料口和外层加料口填充到成型模具内时,并逐渐将双层加料漏斗上提,当造粒粉A和造粒粉B填充到成型模具90~95%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满。
优选地,所述颗粒状造孔剂为400~2000目的壳类活性炭、500~2000目的木质类活性炭、325~2000目的煤质活性炭或3~50μm的有机高分子造孔剂中的一种或其多种的混合物。
优选地,所述壳类活性炭为花生壳或椰子壳活性炭;所述木质类活性炭为木材或竹材活性炭:所述有机高分子造孔剂为PPA、PMMA、PS中的一种或其两种以上的混合物。
优选地,所述种植体外侧壁上设置有外螺纹;所述种植体下端两侧分别设置有止转口,通过口腔细胞增生到止转口内限制外螺纹回转。
优选地,步骤S2中干压压力为6.0~8.0MPa,保压时间为10~30s。
优选地,所述所述步骤S2中冷等静压压力为50~120MPa,保压时间为300~600s。
优选地,步骤S3中素坯的具体烧结方法为:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温40-90min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体。
采用上述技术方案后,本发明与背景技术相比,具有如下有益效果:
1、本发明中造粒粉A和造粒粉B的主要成分均为3mol%钇稳定氧化锆粉,区别为在作为表面材料的造粒粉B中添加了颗粒状造孔剂,所以造粒粉A和造粒粉B的结合性好,通过分层加料后,可同步成型,烧结制得的种植体既能保持氧化锆良好的力学性能,又能保证种植体牙根部表面具有人体牙根相近的孔隙,克服了喷涂、喷丸处理工艺制备的种植体表面与主体结合不牢固及喷砂工艺制备的种植体对孔隙控制性差的缺点。
2、本发明中由于从利于烧成和固相反应进行的角度考虑,采用超细的氧化锆和氧化钇原料颗粒,但粉料越细,比表面积越大,流动性越差,干压成型时不容易均匀的充满模具,经常出现成型件有空洞、边角不致密、层裂、弹性失效的问题,因此通过造粒工艺制成流动性好、粒径为0.06-0.15mm的颗粒。
3、本发明采用分段升温烧结的方式,防止烧结过程中种植体出现裂纹以及对种植体表面的损坏,将升温、保温和再升温过程结合,使得种植体内部均匀受热,能够烧透,可保证种植体结构稳定,同时在烧结的过程中,活性炭类或有机高分子颗粒状造孔剂被燃烧,在种植体表面层形成均匀有序的孔隙,且在干压或冷等静压成型过程中,接触的造粒粉A和造粒粉B会互相渗透,形成渐变的过渡层,在孔隙率提高的同时,还具有较高的抗压强度。
4、本发明先用去离子水清洗坯体表面的杂质,再用盐酸浸泡,除去孔隙内残留的积炭,再用NaHCO3溶液中和多余的盐酸,最后用去离子水再次清洗,可充分除去种植体孔隙中的残留物。
5、本发明制得的种植体表面不仅具有许多孔隙,还具有螺纹和止转口,后期口腔细胞增生到孔隙、螺纹槽和止转口内后,不但可有效限制种植体发生转动,而且可提高种植体的抗拔能力。
附图说明
图1为本发明的种植体的仰视立体结构示意图;
图2为本发明的种植体的前视立体结构示意图;
图3为本发明的双层加料漏斗的立体结构示意图;
图4为本发明的双层加料漏斗的剖切结构示意图;
图5为本发明的另一种双层加料方法的结构示意图。
图中附图标记表示为:
1、种植体;11、外螺纹;12、止转口;2、双层加料漏斗;21、中间加料口;22、外层加料口。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
参见图1至图5所示,一种陶瓷种植体的制备方法,包括以下具体步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.1mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉70份和1200目的花生壳活性炭30份混合均匀,再经过造粒机制成粒径为0.1mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,即采用具有同心加料口的双层加料漏斗2,先将双层加料漏斗2伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗2的中间加料口21和外层加料口22填充到成型模具内时,并逐渐将双层加料漏斗2上提,当造粒粉A和造粒粉B填充到成型模具92%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满,表面层的厚度为总厚度的22%,经干压成型后得到毛坯,其中干压压力为7.5MPa,保压时间为20s,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温60min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡4h,然后20%NaHCO3溶液浸泡1.5h,最后用去离子水清洗;
S5、杀菌,将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
实施例2
参见图1至图3所示,一种陶瓷种植体的制备方法,包括以下具体步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.1mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉70份和1400目的竹材活性炭30份混合均匀,再经过造粒机制成粒径为0.1mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,即采用具有同心加料口的双层加料漏斗2,先将双层加料漏斗2伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗2的中间加料口21和外层加料口22填充到成型模具内时,并逐渐将双层加料漏斗2上提,当造粒粉A和造粒粉B填充到成型模具92%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满,表面层的厚度为表面层和中间层总厚度的22%,经干压成型后得到毛坯,其中干压压力为7.5MPa,保压时间为20s,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温60min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡4h,然后20%NaHCO3溶液浸泡1.5h,最后用去离子水清洗;
S5、杀菌,将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
实施例3
参见图1至图3所示,一种陶瓷种植体的制备方法,包括以下具体步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.1mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉70份和1000目的煤质活性炭30份混合均匀,再经过造粒机制成粒径为0.1mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,即采用具有同心加料口的双层加料漏斗2,先将双层加料漏斗2伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗2的中间加料口21和外层加料口22填充到成型模具内时,并逐渐将双层加料漏斗2上提,当造粒粉A和造粒粉B填充到成型模具92%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满,表面层的厚度为表面层和中间层总厚度的22%,经干压成型后得到毛坯,其中干压压力为7.5MPa,保压时间为20s,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温60min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡4h,然后20%NaHCO3溶液浸泡1.5h,最后用去离子水清洗;
S5、杀菌,将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
实施例4
参见图1至图3所示,一种陶瓷种植体的制备方法,包括以下具体步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.1mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉70份和35μm的PPA树脂30份混合均匀,再经过造粒机制成粒径为0.1mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,即采用具有同心加料口的双层加料漏斗2,先将双层加料漏斗2伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗2的中间加料口21和外层加料口22填充到成型模具内时,并逐渐将双层加料漏斗2上提,当造粒粉A和造粒粉B填充到成型模具92%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满,表面层的厚度为表面层和中间层总厚度的22%,经干压成型后得到毛坯,其中干压压力为7.5MPa,保压时间为20s,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温60min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡4h,然后20%NaHCO3溶液浸泡1.5h,最后用去离子水清洗;
S5、杀菌,将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求的保护范围为准。
Claims (8)
1.一种陶瓷种植体的制备方法,其特征在于,包括以下步骤:
S1、配料:将3mol%钇稳定氧化锆粉经过造粒机制成粒径为0.06-0.15mm的造粒粉A;按重量比将3mol%钇稳定氧化锆粉60-80份、造孔剂20-40份混合均匀,再经过造粒机制成粒径为0.06-0.15mm的造粒粉B;
S2、成型:采用双层加料方法同时将造粒粉A和造粒粉B分别填充到成型模具的中间层和四周的表面层中,表面层的厚度为总厚度的20%-25%,经干压或冷等静压成型后得到毛坯,成型后的毛坯经去毛刺、调尺寸的修坯加工后得到素坯;
S3、烧结:将常温的素坯放入烧结炉中,素坯经过分段升温后,在1500-1530℃的温度条件下保温40-90min,得到坯体,并将坯体加工至所需尺寸;
S4、酸洗:将烧结好的坯体先用去离子水清洗,再用15%盐酸浸泡3-5h,然后20%NaHCO3溶液浸泡1~2h,最后用去离子水清洗;
S5、杀菌:将清洗好的坯体烘干、杀菌,最终制得陶瓷种植体。
2.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于,步骤S2中的双层加料方法具体为:采用具有同心加料口的双层加料漏斗,先将双层加料漏斗伸入成型模具底部,再将造粒粉A和造粒粉B分别从双层加料漏斗的中间加料口和外层加料口填充到成型模具内时,并逐渐将双层加料漏斗上提,当造粒粉A和造粒粉B填充到成型模具90~95%高度时,继续填充造粒粉B,停止填充造粒粉A,直至将成型模具填满。
3.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于:所述颗粒状造孔剂为400~2000目的壳类活性炭、500~2000目的木质类活性炭、325~2000目的煤质活性炭或3~50μm的有机高分子造孔剂中的一种或其多种的混合物。
4.如权利要求3所述的一种陶瓷种植体的制备方法,其特征在于:所述壳类活性炭为花生壳或椰子壳活性炭;所述木质类活性炭为木材或竹材活性炭:所述有机高分子造孔剂为PAA、PMMA、PS中的一种或其两种以上的混合物。
5.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于:所述种植体外侧壁上设置有外螺纹;所述种植体下端两侧分别设置有止转口,通过口腔细胞增生到止转口内限制外螺纹回转。
6.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于:步骤S2中干压压力为6.0~8.0MPa,保压时间为10~30s。
7.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于:所述所述步骤S2中冷等静压压力为50~120MPa,保压时间为300~600s。
8.如权利要求1所述的一种陶瓷种植体的制备方法,其特征在于,步骤S3中素坯的具体烧结方法为:将常温的素坯放入烧结炉中,经60min将温度升至320℃后,保温120min;保温结束后,经160min将温度继续升至800℃后,保温150min;保温结束后,经300min将温度继续升至1200℃后,保温40min;保温结束后,经300min将温度继续升至1500℃后,保温40-90min;保温结束后,经400min将温度降至700℃后,再自然冷却至室温得到坯体。
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